Bromoacetyl chloride → 3-Methyl-6-(bromoacetyl)benzothiazolinone

HRID 326239ノート

反応式

HRID 326239 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[S:8](=[O:15])[CH2:7]1.[Br:16][CH2:17][C:18](Cl)=[O:19]>CN(C)C=O>[CH3:5][N:6]1[C:10]2[CH:11]=[CH:12][C:13]([C:18](=[O:19])[CH2:17][Br:16])=[CH:14][C:9]=2[S:8](=[O:15])[CH2:7]1

参加物

5

反応物 3

HCID 89602Bromoacetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 20026384N-methylbenzothiazolone

生成物 1

HCID 867466573-Methyl-6-(bromoacetyl)benzothiazolinone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

210 g (1.60 mol) of aluminum chloride are introduced into a 500-cm3 ground-necked flask surmounted by a condenser, and 43 cm3 of dimethylformamide are then added dropwise and with magnetic stirring via a dropping funnel. 33 9 (0.20 mol) of 3-methylbenzothiazolinone are then added and, while the reaction medium homogenizes, the temperature is stabilized at 70° C. using an oil bath. 19.8 cm3 (0.24 mol) of bromoacetyl chloride are then added gradually. After the addition, the mixture is left stirring for one hour at a temperature of 70° C. The reaction medium is hydrolyzed by pouring it onto crushed ice and the precipitate obtained is drained, washed with water until the filtrate is neutral and dried. The product is recrystallized in 95° strength alcohol.

後処理

  1. customsurmounted by a condenser
  2. customis stabilized at 70° C.
  3. additionAfter the addition
  4. waitthe mixture is left
  5. stirringstirring for one hour at a temperature of 70° C
  6. additionby pouring it
  7. customonto crushed ice
  8. customthe precipitate obtained
  9. washwashed with water until the filtrate
  10. customdried
  11. customThe product is recrystallized in 95° strength alcohol

出典と根拠

ORDレコード
ord-0c988c1e91dc4f7391d8a4b11cfe06e4
出典データセット
uspto-grants-1993_12
特許番号
US05268381

反応ノート

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