Реакция #2324520

Уравнение реакции

NaOH

4-chlorobutanoyl chloride

cystamine hydrochloride

NaOH

→

N,N′-(disulfanediyldiethane-2,1-diyl)bis(4-chlorobutanamide)

Растворители

THF

Условия реакции

Обработка

1. 1
   workup.ADDITIONAfter completion of the addition and stabilization of pH at 7
2. 2
   workup.ADDITIONthe mixture mixed for 3 days
3. 3
   ЭкстракцияThe aqueous layer was extracted with 3×500 mL dichloromethane
4. 4
   Сушкаdried over Na2SO4
5. 5
   СушкаAfter drying under vacuum, 41 g of a white powder
6. 6
   Другоеwere collected

Методика

60 g of cystamine hydrochloride was solubilized in 500 mL and cooled to 5° C. The pH was raised to 10 by addition of aq. NaOH (30%). A solution of 4-chlorobutanoyl chloride (105 g) in anhydrous THF (500 mL), was added dropwise, while the pH was maintained above 7 by addition of aq. NaOH (30%). After completion of the addition and stabilization of pH at 7, the mixture mixed for 3 days. The aqueous layer was extracted with 3×500 mL dichloromethane, combined with THF layer and dried over Na2SO4. After drying under vacuum, 41 g of a white powder were collected. Analyses were in accordance with the expected structure.

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