Water → HCID 54109521, 화합물

HRID 258700노트

반응식

HRID 258700 반응식
[H-].[Na+].[S:3]([C:7]1[NH:8][CH:9]=[CH:10][N:11]=1)([CH3:6])(=[O:5])=[O:4].Cl[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15].O>CN(C)C=O.C(Cl)Cl>[S:3]([C:7]1[N:8]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:9]=[CH:10][N:11]=1)([CH3:6])(=[O:5])=[O:4]

참가 물질

7

반응물 4

HCID 962WaterHCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 993902-(Methylsulfonyl)imidazole

생성물 1

HCID 54109521HCID 54109521, 화합물수율 88%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
20 °C

실험 절차

Sodium hydride (50% suspension in mineral oil) (5.04 g.) is added, under a nitrogen atmosphere, to a solution of 2-mesyl-imidazole (15.3 g.) in dimethylformamide (130 cc.). Ethyl chloroacetate (12.9 g.) is then added. Reaction is allowed to take place for 20 hours, with stirring, at a temperature of about 20° C. The reaction mixture is then poured into water (4 liters) and extraction is effected using methylene chloride (1 liter). The methylene chloride extracts are washed with water, dried over sodium sulphate, treated with decolorising charcoal and then concentrated to dryness under reduced pressure (0.5 mm.Hg) to yield ethyl (2-mesyl-imidazol-1-yl)-acetate (21.4 g.) in the form of an oil.

후처리

  1. customReaction
  2. customfor 20 hours
  3. washThe methylene chloride extracts are washed with water
  4. dry with materialdried over sodium sulphate
  5. additiontreated with decolorising charcoal
  6. concentrationconcentrated to dryness under reduced pressure (0.5 mm.Hg)

출처 및 근거

ORD 기록
ord-8d03edfc897a427fbd339f239b7ac215
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04034088

반응 노트

불러오는 중…