Hydrochloric Acid → HCID 22760436、化合物

HRID 461193ノート

反応式

HRID 461193 の反応式
[Br:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([S:12](=[O:17])(=[O:16])[N:13]([CH3:15])[CH3:14])[CH:6]=1)=[O:4].[BH4-].[Na+].Cl>CO>[Br:1][CH2:2][CH:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([S:12](=[O:16])(=[O:17])[N:13]([CH3:14])[CH3:15])[CH:6]=1)[OH:4]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 204768462-Bromo-4'-chloro-3'-dimethylsulfamoylacetophenone

生成物 1

HCID 22760436HCID 22760436、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 6.4 g of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone in 28 ml of methanol were added dropwise, at a reaction temperature of 5° C, a solution of 0.6 g of sodium borohydride in 5 ml of methanol and the solution was then stirred for 1 hour at room temperature. The reaction mixture was acidified while cooling (+5° C) with 2 N HCl and the solvent was distilled off under reduced pressure. After adding 70 ml of water, extraction followed with 200 ml of diethyl ether, the organic phase was dried over sodium sulfate, the solvent was distilled off and 2-bromo-1-(4-chloro-3-dimethylsulfamoylphenyl)-ethanol was obtained as fair yellow to colorless oil.

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionAfter adding
  3. extraction70 ml of water, extraction
  4. dry with materialthe organic phase was dried over sodium sulfate
  5. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-5385b662ef2049898848fabaecbbb030
出典データセット
uspto-grants-1977_12
特許番号
US04061761

反応ノート

読み込み中…