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

HRID 979309ノート

反応式

HRID 979309 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.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]

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 129.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-910e31368f7841b597278a48f33dfee3
出典データセット
uspto-grants-1987_05
特許番号
US04667032

反応ノート

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