Sodium Dithionite → 4-bromo-2,7-dimethoxy-3-hydroxy-10H-phenothiazine

HRID 979309노트

반응식

HRID 979309 반응식
[Br:1][C:2]1[C:3](=[O:20])[C:4]([O:18][CH3:19])=[CH:5][C:6]2[C:15]=1[S:14][C:13]1[C:8](=[CH:9][CH:10]=[C:11]([O:16][CH3:17])[CH:12]=1)[N:7]=2.S(S([O-])=O)([O-])=O.[Na+].[Na+]>C(OCC)(=O)C.O>[Br:1][C:2]1[C:15]2[S:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:16][CH3:17])[CH:12]=3)[NH:7][C:6]=2[CH:5]=[C:4]([O:18][CH3:19])[C:3]=1[OH:20]

참가 물질

5

반응물 2

HCID 24489Sodium DithioniteHCID 1221824-Bromo-2,7-dimethoxy-3H-phenothiazin-3-one

생성물 1

HCID 138537384-bromo-2,7-dimethoxy-3-hydroxy-10H-phenothiazine수율 129.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of 4-bromo-2,7-dimethoxy-3H-phenothiazin-3-one (100 g) in a mixture of ethyl acetate (2 l) and water (1 l) was added sodium hydrosulfite (200 g) in one batch with mechanical stirring. The orange reaction mixture was stirred for 15 hours under a nitrogen atmosphere. The resulting white reaction mixture was filtered and the precipitate washed with water under a nitrogen atmosphere to prevent air oxidation of the compound. The title compound (130 g) was obtained as a wet material and was used as such in the next step (Step 2). An analytical sample was air dried, m.p. 185° C.

후처리

  1. filtrationThe resulting white reaction mixture was filtered
  2. washthe precipitate washed with water under a nitrogen atmosphere

출처 및 근거

ORD 기록
ord-910e31368f7841b597278a48f33dfee3
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04667032

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