Hydrochloric Acid → Methanesulfonamide, N-[4-(2-chloroacetyl)phenyl]-

HRID 65238

反応式

HRID 65238 の反応式
[C:1]1([NH:7][S:8]([CH3:11])(=[O:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:12][CH2:13][C:14](Cl)=[O:15].[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(Cl)Cl>[Cl:12][CH2:13][C:14]([C:4]1[CH:3]=[CH:2][C:1]([NH:7][S:8]([CH3:11])(=[O:10])=[O:9])=[CH:6][CH:5]=1)=[O:15]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 70970Methanesulfonamide, N-phenyl-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 116629Methanesulfonamide, N-[4-(2-chloroacetyl)phenyl]-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

In a flask containing 128.4 g (0.75 mole) of N-phenylmethanesulfonamide, 169.5 g (1.50 mole) of chloroacetyl chloride in 1 L of methylene chloride under an atmosphere of nitrogen and cooled to about -10° C. add 300 g (2.25 mole) of aluminum chloride. Stir the resulting mixture for about 2 hours at -10° C. then warm to room temperature for about 16 hours. Pour the reaction mixture onto 2 Kg of ice containing 600 mL of concentrated hydrochloric acid. Collect the precipitate and wash with methanol (3×300 mL) and dry in vacuo to give the title compound.

後処理

  1. temperaturethen warm to room temperature for about 16 hours
  2. customCollect the precipitate
  3. washwash with methanol (3×300 mL)
  4. customdry in vacuo

出典と根拠

ORDレコード
ord-b24a3c0eee3e49658076d6d493e15730
出典データセット
uspto-grants-1986_09
特許番号
US04613609

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