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

HRID 231057노트

반응식

HRID 231057 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.[O-]S(S([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 79.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

The compound from Step 4 (300 mg) was suspended in ethyl acetate (100 ml) and a solution of Na2S2O4 (2 g) in water (40 ml) was then added and the mixture was shaken until the orange-red coloration disappeared. The aqueous layer was decanted, the organic layer was washed with water, dried and evaporated to dryness. The resulting residue was treated with ether and filtered to afford the title compound (240 mg), m.p. 185° C.

후처리

  1. customThe aqueous layer was decanted
  2. washthe organic layer was washed with water
  3. customdried
  4. customevaporated to dryness
  5. additionThe resulting residue was treated with ether
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-4a252d00919a4e7fa649118b66d057e6
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845083

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