Hexane → 4-Bromo-7-methoxy-2-(4-methylpiperazin-1-yl)-3H-phenothiazin-3-one

HRID 979308ノート

反応式

HRID 979308 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:14](=[CH:15][CH:16]=1)[N:13]=[C:12]1[C:7](=[CH:8][C:9](=[O:24])[C:10]([N:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)=[CH:11]1)[S:6]2.[Br:25]Br.CCCCCC>C(O)(=O)C>[Br:25][C:8]1[C:9](=[O:24])[C:10]([N:17]2[CH2:18][CH2:19][N:20]([CH3:23])[CH2:21][CH2:22]2)=[CH:11][C:12]2[C:7]=1[S:6][C:5]1[C:14](=[CH:15][CH:16]=[C:3]([O:2][CH3:1])[CH:4]=1)[N:13]=2

参加物

5

反応物 3

HCID 8058HexaneHCID 24408BromineHCID 138537347-Methoxy-2-(4-methylpiperazin-1-yl)-3H-phenothiazine-3-one

生成物 1

HCID 138537354-Bromo-7-methoxy-2-(4-methylpiperazin-1-yl)-3H-phenothiazin-3-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a suspension of 7-methoxy-2-(4-methylpiperazin-1-yl)-3H-phenothiazin-3-one (500 mg) in acetic acid (10 ml) was added a solution of bromine in acetic acid (0.5M) (6 ml) and stirred for 5 minutes. Hexane (100 ml) was added and the resulting precipitate was filtered. The solid was suspended in a mixture of aqueous K2CO3 (50 ml), EtOAc (100 ml) and methanol (20 ml) and stirred for 15 minutes. After filtration and decantation, the organic layer was washed with brine, dried and evaporated to dryness to afford the title compound (190 mg) m.p. 209°-210° (dec.).

後処理

  1. filtrationthe resulting precipitate was filtered
  2. additionThe solid was suspended in a mixture of aqueous K2CO3 (50 ml), EtOAc (100 ml) and methanol (20 ml)
  3. stirringstirred for 15 minutes
  4. filtrationAfter filtration and decantation
  5. washthe organic layer was washed with brine
  6. customdried
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-83c87d3c314b4c51a44c41ab61e687ff
出典データセット
uspto-grants-1987_05
特許番号
US04667032

反応ノート

読み込み中…