m-Chloroperbenzoic acid → 5-Acetoxy-12H-benzo[a]phenothiazine-7-oxide

HRID 2352228노트

반응식

HRID 2352228 반응식
[C:1]([O:4][C:5]1[CH:18]=[C:17]2[C:8]([NH:9][C:10]3[C:15]([S:16]2)=[CH:14][CH:13]=[CH:12][CH:11]=3)=[C:7]2[CH:19]=[CH:20][CH:21]=[CH:22][C:6]=12)(=[O:3])[CH3:2].ClC1C=C(C=CC=1)C(OO)=[O:28]>ClCCl.CO>[C:1]([O:4][C:5]1[CH:18]=[C:17]2[C:8]([NH:9][C:10]3[C:15]([S:16]2=[O:28])=[CH:14][CH:13]=[CH:12][CH:11]=3)=[C:7]2[CH:19]=[CH:20][CH:21]=[CH:22][C:6]=12)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 137124795-acetoxy-12H-benzo[a]phenothiazine

생성물 1

HCID 137124815-Acetoxy-12H-benzo[a]phenothiazine-7-oxide

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a suspension of 5-acetoxy-12H-benzo[a]phenothiazine (10 g) in dichloromethane (125 cc) there was raidly added a solution of 85% m-chloroperoxybenzoic acid (6.61 g) in methanol (125 ml). At first the solids dissolved, then after a few minutes a new solid separated out of solution. After 1 and 1/2 hours the mixture was filtered and the solid washed with dichloromethane. The title compound was thus obtained pure (8.76 g), m.p. 179°-181° C.

후처리

  1. dissolutionAt first the solids dissolved
  2. customafter a few minutes a new solid separated out of solution
  3. filtrationAfter 1 and 1/2 hours the mixture was filtered
  4. washthe solid washed with dichloromethane

출처 및 근거

ORD 기록
ord-044291c03d0e4acf9b3b1b960156c7e7
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04876246

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