Water → HCID 54109521、化合物

HRID 258700ノート

反応式

HRID 258700 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 54109521HCID 54109521、化合物収率 88%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8d03edfc897a427fbd339f239b7ac215
出典データセット
uspto-grants-1977_07
特許番号
US04034088

反応ノート

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