Benzisothiazole → 3-Chloro-1,2-benzisothiazole

HRID 341976

反応式

HRID 341976 の反応式
C[S:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH:5]=[N:6]O.S(Cl)([Cl:14])=O.ClCl.S1C2C=CC=CC=2C=N1>ClC1C=CC=CC=1>[Cl:14][C:5]1[C:4]2[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=2[S:2][N:6]=1

参加物

6

反応物 4

HCID 9225BenzisothiazoleHCID 24386Thionyl ChlorideHCID 24526ChlorineHCID 7867572-(Methylthio)benzaldehyde oxime

生成物 1

HCID 5981903-Chloro-1,2-benzisothiazole収率 96.1%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

In a 300 ml four-necked flask equipped with a stirrer, a thermometer, and a condenser, 100 g of monochlorobenzene was placed in advance, to which 33.4 g (0.2 mol) of 2-(methylthio)benzaldehyde oxime was added under nitrogen atmosphere. 25.2 g (0.21 mol) Of thionyl chloride was added dropwise thereto while stirring at a temperature of from -10° to -15° C. and allowed to react for 1 hour at the same temperature. After the termination of the reaction, 15.6 g (0.22 mol) of chlorine was continuously blown into the reaction mixture containing 1,2-benzisothiazole while stirring at a temperature of from 70° to 80° C. and allowed to react for 1 hour at the same temperature. After the termination of the reaction, the reaction mixture was subjected to distilling off of the solvent and then to distillation under reduced pressure to give 32.6 g of 3-chloro-1,2-benzisothiazole. The yield was 96% to the 2-(methylthio)benzaldehyde oxime.

後処理

  1. customIn a 300 ml four-necked flask equipped with a stirrer
  2. additionwas added under nitrogen atmosphere
  3. customto react for 1 hour at the same temperature
  4. stirringwhile stirring at a temperature of from 70° to 80° C.
  5. customto react for 1 hour at the same temperature
  6. customAfter the termination of the reaction
  7. distillationto distilling off of the solvent
  8. distillationto distillation under reduced pressure

出典と根拠

ORDレコード
ord-5452ffc334694ae09b9bc88857992547
出典データセット
uspto-grants-1999_01
特許番号
US05856504

関連ノート

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