1-Phenethylamine, (-)- → HCID 67062310、化合物

HRID 1268735ノート

反応式

HRID 1268735 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[N:9]=[C:10]([CH2:20][CH3:21])[S:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[C:15](F)[CH:14]=2)[CH:5]=[CH:6][CH:7]=1.[C:22]1([C@@H:28]([NH2:30])[CH3:29])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(=O)([O-])O.[Na+]>>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[N:9]=[C:10]([CH2:20][CH3:21])[S:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[C:15]([NH:30][C@H:28]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH3:29])[CH:14]=2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 758181-Phenethylamine, (-)-HCID 516892Sodium BicarbonateHCID 178629784-(3-Chlorophenyl)-2-ethyl-5-(2-fluoro-4-pyridyl)-1,3-thiazole

生成物 1

HCID 67062310HCID 67062310、化合物収率 107.6%

反応条件

温度
150 °C

実験手順

A mixture of 4-(3-chlorophenyl)-2-ethyl-5-(2-fluoro-4-pyridyl)-1,3-thiazole (0.35 g, 1.1 mmol) and (S)-1-phenylethylamine (1.4 mL, 11 mmol) was stirred at 150° C. for 16 hrs. The reaction mixture was cooled to room temperature, saturated aqueous sodium hydrogen carbonate solution was added and the mixture was extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The obtained oil was treated with 10% hydrogen chloride-methanol to give the title compound (0.27 g, yield 56%).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. additionThe obtained oil was treated with 10% hydrogen chloride-methanol

出典と根拠

ORDレコード
ord-495e3c80e77545efa9ccd6d17df3487f
出典データセット
uspto-grants-2007_04
特許番号
US07199124B2

反応ノート

読み込み中…