Acetic Acid → 7-Acetamino-4-acetoxy-1,2-benzisothiazole

HRID 1449117ノート

反応式

HRID 1449117 の反応式
[N+:1]([C:4]1[C:12]2[S:11][N:10]=[CH:9][C:8]=2[C:7]([OH:13])=[CH:6][CH:5]=1)([O-])=O.[C:14]([OH:17])(=O)[CH3:15].[H][H].[C:20](OC(=O)C)(=[O:22])[CH3:21]>[Pd]>[NH:1]([C:4]1[C:12]2[S:11][N:10]=[CH:9][C:8]=2[C:7]([O:13][C:14](=[O:17])[CH3:15])=[CH:6][CH:5]=1)[C:20]([CH3:21])=[O:22]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 1357653737-Nitro-4-hydroxy-1,2-benzisothiazoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 203499417-Acetamino-4-acetoxy-1,2-benzisothiazole収率 67%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

5.0 g of 7-nitro-4-hydroxy-1,2-benzisothiazole, in a mixture of 50 ml of acetic anhydride, 10 ml of acetic acid and 50 mg of a 5% strength palladium-on-charcoal catalyst, are left for 10 hours at 60° C. under 100 bars hydrogen pressure. After the mixture has cooled, the catalyst is filtered off, the filtrate is concentrated under reduced pressure and the partially crystalline crude product is recrystallized from acetic anhydride. 4.2 g (67% of theory) of 7-acetamino-4-acetoxy-1,2-benzisothiazole of melting point 215°-216° C. are obtained.

後処理

  1. temperatureAfter the mixture has cooled
  2. filtrationthe catalyst is filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customthe partially crystalline crude product is recrystallized from acetic anhydride

出典と根拠

ORDレコード
ord-16499a6ed4064bd39bd7dfdcf0158228
出典データセット
uspto-grants-1980_02
特許番号
US04189433

反応ノート

読み込み中…