Iodoethane → 10-(1-Diethylamino-2-propyl)-2-phenothiazinecarbonitrile

HRID 704196ノート

反応式

HRID 704196 の反応式
[CH2:1]([NH:3][CH2:4][CH:5]([N:7]1[C:20]2[CH:19]=[C:18]([C:21]#[N:22])[CH:17]=[CH:16][C:15]=2[S:14][C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH3:6])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].I[CH2:30][CH3:31]>CN(C)C=O>[CH2:1]([N:3]([CH2:30][CH3:31])[CH2:4][CH:5]([N:7]1[C:20]2[CH:19]=[C:18]([C:21]#[N:22])[CH:17]=[CH:16][C:15]=2[S:14][C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH3:6])[CH3:2]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 10340Sodium CarbonateHCID 14536548HCID 14536548、化合物

生成物 1

HCID 1453650710-(1-Diethylamino-2-propyl)-2-phenothiazinecarbonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

A mixture of 10-(1-ethylamino-2-propyl)-2-phenothiazinecarbonitrile acid fumarate, D series (4 g), sodium carbonate (1.32 g) and iodoethane (1 cc) in dimethylformamide (50 cc) is heated to a temperature in the region of 150° C. for 6 hours. After cooling, the reaction mixture is concentrated to dryness (30 m Hg; 4 kPa) at 50° C. and the residue is taken up with ethyl acetate (100 cc) and washed successively with distilled water (50 cc) and with saturated aqueous sodium chloride solution (50 cc). The organic phase is dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. 10-(1-diethylamino-2-propyl)-2-phenothiazinecarbonitrile, D series (3.4 g) is thereby obtained in the form of a yellow oil.

後処理

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture is concentrated to dryness (30 m Hg; 4 kPa) at 50° C.
  3. washwashed successively with distilled water (50 cc) and with saturated aqueous sodium chloride solution (50 cc)
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C

出典と根拠

ORDレコード
ord-e4ea84fe2a034bd0a2478a29e730ca59
出典データセット
uspto-grants-1991_01
特許番号
US04985419

反応ノート

読み込み中…