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

HRID 979091ノート

反応式

HRID 979091 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 138537384-bromo-2,7-dimethoxy-3-hydroxy-10H-phenothiazine収率 79.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e446a3ee50074fa996e26fa51691a3f4
出典データセット
uspto-grants-1987_05
特許番号
US04666907

反応ノート

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