Sodium Cyanoborohydrideyog ib qho organic compound uas yuav siv tau los txo cov acyl tebchaw thiab lwm cov organic tebchaw, yog li nws yog ib qho ntawm cov feem ntau siv txo cov neeg ua haujlwm hauv cov organic synthesis. Cov hauv qab no yog ob txoj kev siv hluavtaws ntawm Sodium Cyanoborohydride:
1. Cov tshuaj tiv thaiv sodium cyanide thiab sodium borohydride
Sodium cyanide thiab sodium borohydride yog thawj zaug sib xyaw thiab hnov qab ntawm chav tsev kub. Sodium Cyanoborohydride thiab hydrogen yog tsim thaum lub sij hawm cov tshuaj tiv thaiv:
NaCN plus NaBH4→ NAB3CN plus H2
Tom qab cov tshuaj tiv thaiv, qhov tshwm sim Sodium Cyanoborohydride tuaj yeem tau los ntawm kev lim thiab ziab hauv qab nqus kom tau txais cov khoom ntshiab.
Cov kauj ruam ntxaws ntxaws ntawm cov tshuaj tiv thaiv yog raws li nram no:
(1) Hauv qhov chaw qhuav, sib tov sodium cyanide thiab sodium borohydride ntawm molar ratio ntawm 1: 1, thiab ntxiv cov sib tov kom qhuav anhydrous methanol.
(2) Ntxiv methanol sib tov rau hauv lub reactor thiab cua sov rau cov tshuaj tiv thaiv kub nrog nplawm. Feem ntau cov tshuaj tiv thaiv kub yog 0-5 degree , uas tuaj yeem tswj tau nrog da dej khov nab kuab.
(3) Maj mam ntxiv qhov tsim nyog ntawm cov dej dropwise rau cov tshuaj tiv thaiv sib tov los txhawb cov tshuaj tiv thaiv. Thaum lub sij hawm cov tshuaj tiv thaiv, methanol decomposes formaldehyde thiab hydrogen gas, thaum sodium cyanide thiab sodium borohydride reacts rau daim ntawv NaBH3CN.
(4) Tom qab cov tshuaj tiv thaiv tiav, cov tshuaj tiv thaiv sib tov yog lim kom tshem tawm cov khoom seem, thiab tom qab ntawd cov khoom raug ntxuav nrog dej lossis methanol.
2. Cov tshuaj tiv thaiv sodium cyanide thiab boron trichloride
Sodium cyanide thiab boron trichloride yog thawj zaug sib xyaw thiab tshwm sim ntawm chav tsev kub. Cov tshuaj tiv thaiv tsim cov cyanide thiab hydrogen, thiab tsim cov tshuaj nruab nrab sodium trichloride borocyanide (NaCN·BCl3). Tom qab ntawd, sulfuric acid tau ntxiv, qhov nruab nrab yog hydrolyzed thiab qhuav hauv lub tshuab nqus tsev kom muab Sodium Cyanoborohydride:
NaCN plus BCl3→ NaCN BCl3
NAS BCl3ntxiv H2O plus H2YOG4→ NAB3CN plus H3BO3plus NaHSO4
Cov txheej txheem tshuaj tiv thaiv yog qhov yooj yim, cov kauj ruam yog raws li nram no:
(1) Sib tov sodium cyanide thiab boron trichloride ntawm molar ratio ntawm 1: 1, thiab ntxiv ib tug txaus npaum li cas ntawm acetonitrile, DMF los yog DMSO thiab lwm yam organic solvents.
(2) Maj mam ntxiv dilute acid (xws li HCl lossis H2YOG4) mus rau cov tshuaj tiv thaiv sib tov nyob rau hauv nplawm, thiab nws tuaj yeem pom tias qhov sib xyaw ua ke hloov mus rau hauv kev tshem tawm dawb thaum cov tshuaj tiv thaiv.
(3) Cov tshuaj tiv thaiv feem ntau yog ua los ntawm chav tsev kub, thiab dej txias lossis dej khov tuaj yeem siv los tswj qhov kub thiab txias, thiab cov tshuaj tiv thaiv feem ntau yuav siv sijhawm 2-4 teev.
(4) Tom qab cov tshuaj tiv thaiv tiav, dilute cov tshuaj tiv thaiv sib tov nrog dej, tom qab ntawd ntxuav cov khoom nrog cov tshuaj ntsev inorganic (xws li sodium acetate tov), thiab thaum kawg ntxuav nrog ethanol.
(5) Qhuav cov khoom ntxuav kom tau txais NaBH siab3CN.
Ob txoj hauv kev saum toj no tuaj yeem npaj Sodium Cyanoborohydride, tab sis thawj txoj kev yooj yim dua, yog li nws muaj ntau dua hauv chav kuaj.
Nov yog qee txoj hauv kev siv hluavtaws rau kev sib xyaw ntawm Sodium cyanoborohydride:
1. Boron trichloride txoj kev:
Tom qab sib tov sodium borate thiab hydrocyanic acid, boron trichloride ntxiv thiab rhuab kom tau NaBH3CN.
Ua raws li hauv qab no:
(1) Nyob rau hauv ib qho chaw qhuav, sib tov boron trichloride thiab methanol ntawm molar ratio ntawm 1: 1.
(2) Maj mam ntxiv hydrocyanic acid nyob rau hauv stirring tej yam kev mob, thiab cov tshuaj tiv thaiv sib tov yuav tsim boron cyanide. Thaum lub sij hawm cov tshuaj tiv thaiv, qhov sib tov tau pom tau hloov los ntawm tsaus liab mus rau txiv kab ntxwv thiab tom qab ntawd mus rau lub teeb daj.
(3) Ntxiv sodium cyanide thiab ib qho methanol txaus, thiab txuas ntxiv mus do cov tshuaj tiv thaiv sib tov. Hauv cov kauj ruam no, boron cyanide reacts nrog sodium cyanide los ua NaBH3CN thiab NaCl.
(4) Tom qab cov tshuaj tiv thaiv tiav, cov tshuaj tiv thaiv sib tov yog lim kom tshem tawm cov khoom seem. Tom qab ntawd cov khoom yog ntxuav nrog dej los yog methanol.
(5) Thaum kawg, cov khoom ntxuav tau qhuav kom tau txais NaBH siab3CN.
2. Formaldehyde txoj kev:
Tom qab sib tov formaldehyde thiab hydrocyanic acid, sodium hydroxide yog ntxiv nyob rau hauv qhov kev txiav txim ntawm alkali kom tau NaBH3CN.
Cov kauj ruam tshwj xeeb yog raws li hauv qab no:
(1) Sib tov formaldehyde thiab sodium cyanide ntawm molar ratio ntawm 2: 1, thiab ntxiv ib tug txaus npaum li cas ntawm acetonitrile, DMF los yog DMSO thiab lwm yam organic solvents.
(2) Maj mam ntxiv boron cyanide nyob rau hauv nplawm, feem ntau cov boron cyanide yog 1.2-1.5 npaug ntawm formaldehyde, thiab nws tuaj yeem diluted nrog cov kuab tshuaj organic xws li acetonitrile, DMF lossis DMSO.
(3) Tom qab ntxiv boron cyanide, txuas ntxiv mus do cov tshuaj tiv thaiv sib tov. Cov tshuaj tiv thaiv feem ntau yog ua nyob rau hauv chav tsev kub, thiab pH yuav tsum tau tswj nyob ib ncig ntawm nruab nrab. Lub sijhawm tshuaj tiv thaiv feem ntau yog ob peb teev.
(4) Tom qab cov tshuaj tiv thaiv, cov tshuaj tiv thaiv sib tov yuav diluted nrog dej, thiab cov khoom yog ntxuav nrog ib tug inorganic ntsev tov (xws li sodium acetate tov), thiab thaum kawg ntxuav nrog ethanol.
(5) Qhuav cov khoom ntxuav kom tau txais NaBH siab3CN.
3. Acrylonitrile txoj kev:
Tom qab sib tov acrylonitrile thiab hydrocyanic acid, sodium hydroxide thiab boric acid ntxiv kom tau NaBH3CN.
Cov kauj ruam tshwj xeeb yog raws li hauv qab no:
(1) Sib tov acrylonitrile thiab sodium cyanide ntawm molar piv ntawm 1: 1.5, thiab ntxiv cov kuab tshuaj organic txaus xws li methanol lossis acetonitrile.
(2) Maj mam ntxiv boron cyanide nyob rau hauv nplawm, feem ntau tus nqi ntawm boron cyanide yog 1.2-1.5 npaug ntawm acrylonitrile, thiab nws tuaj yeem diluted nrog cov kuab tshuaj organic.
(3) Tom qab ntxiv boron cyanide, txuas ntxiv mus do cov tshuaj tiv thaiv sib tov. Cov tshuaj tiv thaiv kub yog feem ntau nyob rau hauv chav tsev kub, thiab lub sij hawm cov tshuaj tiv thaiv feem ntau yog ob peb teev.
(4) Tom qab cov tshuaj tiv thaiv, cov tshuaj tiv thaiv sib tov yuav diluted nrog dej, thiab cov khoom yog ntxuav nrog ib tug inorganic ntsev tov (xws li sodium acetate tov), thiab thaum kawg ntxuav nrog ethanol.
(5) Qhuav cov khoom ntxuav kom tau txais NaBH siab3CN.
4. Sodium hydrocyanate txoj kev:
Tom qab sib tov sodium hydrocyanate thiab sodium hydroxide, ntxiv sodium borohydride thiab cua sov rau 60 degree kom tau NaBH3CN.
Cov kauj ruam tshwj xeeb yog raws li hauv qab no:
(1) Sib tov sodium cyanide thiab sodium hydrocyanate hauv qhov sib piv molar ntawm 2: 1, thiab ntxiv dej txaus.
(2) Maj mam ntxiv sodium hydroxide hauv qab nplawm kom txog thaum pH tus nqi ntawm cov tshuaj mus txog 10-11.
(3) Tom ntej no, maj mam ntxiv hydrocyanic acid los tswj tus nqi pH ntawm ib ncig ntawm 7-8, feem ntau yuav tsum tau nplawm tas li thiab cua sov (kwv yees li 60 degree ).
(4) Nyob rau hauv qhov xwm txheej ntawm nplawm thiab cua sov, ntxiv boron cyanide maj mam, feem ntau cov nyiaj boron cyanide yog 1.2-1.5 npaug ntawm hydrocyanic acid, thiab nws tuaj yeem diluted nrog dej.
(5) Tom qab cov tshuaj tiv thaiv, cov khoom tuaj yeem ntxuav nrog cov tshuaj ntsev inorganic (xws li sodium acetate tov), thiab thaum kawg ntxuav nrog ethanol.
(6) Qhuav cov khoom ntxuav kom tau txais NaBH siab3CN.
Ntawm lwm cov txheej txheem hluavtaws, txoj kev boron trichloride yog ib txoj hauv kev siv ntau tshaj plaws. Lwm txoj hauv kev kuj tuaj yeem nqa tawm hauv chav kuaj, tab sis nws yog ib qho tsim nyog yuav tsum xaiv txoj kev tsim nyog tshaj plaws rau kev tsim khoom raws li qhov chaw sim thiab nws cov kev xav tau.