反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
##STR13## In a three necked flask, fitted with a water condenser, a mechanical stirrer and a dropping funnel a solution of 1-bromo-6-cyanohexane (8.04 g, 42.3 mmol) was placed in 75 mL of 95% EtOH. The mixture was heated to reflux and to it was slowly added a solution of sodium sulfite (8.00 g, 63.5 mmol) in 50 mL of H2O over a period of 30 min. The mixture was heated for 2 h and then concentrated under reduced pressure. The residue was dissolved in 95% EtOH (200 ml), heated to boiling and filtered. The filtrate was concentrated and cooled in an ice bath. The precipitate was collected by filtration and dried to give 3.00 g of a white solid. The mother liquor on further concentration, produced another batch of 2.2 g of the product. 1H NMR (300 MHz, DMSO-d6) δ 2.50 (t, j=8 Hz, 2H), 2.40(t, 8 Hz, 2H), 1.55 (m, 4H), 1.3(m, 4H).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux and to it
- temperatureThe mixture was heated for 2 h
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in 95% EtOH (200 ml)
- temperatureheated
- filtrationfiltered
- concentrationThe filtrate was concentrated
- temperaturecooled in an ice bath
- filtrationThe precipitate was collected by filtration
- customdried