Dimethylformamide → HCID 21426439、化合物

HRID 258702ノート

反応式

HRID 258702 の反応式
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[S:7]([C:11]1[N:12]([CH2:16][C:17]([OH:19])=O)[CH:13]=[CH:14][N:15]=1)([CH3:10])(=[O:9])=[O:8].CN(C)C=O>C(Cl)Cl>[S:7]([C:11]1[N:12]([CH2:16][C:17]([Cl:2])=[O:19])[CH:13]=[CH:14][N:15]=1)([CH3:10])(=[O:9])=[O:8]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24819Phosphorus pentachlorideHCID 21426444HCID 21426444、化合物

生成物 1

HCID 21426439HCID 21426439、化合物収率 92.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
10 °C

実験手順

Phosphorus pentachloride (22.5 g.) dissolved in methylene chloride (150 cc.) is added dropwise and whilst cooling to 5° C., to a suspension of (2-mesyl-imidazol-1-yl)-acetic acid (12.3 g.) in methylene chloride (50 cc.). Dimethylformamide (2 cc.) is added thereafter and the mixture is then heated under reflux for 4 hours. The mixture is cooled to 10° C., the resulting solid is filtered off and washed with methylene chloride (15 ac.) to give (2-mesyl-imidazol- 1 -yl)-acetyl chloride (12.4 g.), m.p. 132°-133° C.

後処理

  1. additionis added dropwise
  2. temperaturethe mixture is then heated
  3. temperatureunder reflux for 4 hours
  4. filtrationthe resulting solid is filtered off
  5. washwashed with methylene chloride (15 ac.)

出典と根拠

ORDレコード
ord-bba483467fe846e69d8bc65b5c5bb971
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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