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

HRID 1449117노트

반응식

HRID 1449117 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 203499417-Acetamino-4-acetoxy-1,2-benzisothiazole수율 67%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-16499a6ed4064bd39bd7dfdcf0158228
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04189433

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