Water → Ticlopidine Hydrochloride

HRID 46671

反応式

HRID 46671 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH2:4][NH:5][CH2:6][CH2:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1.Cl[CH2:18]OC.O>CN(C)C=O>[ClH:1].[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH2:4][N:5]1[CH2:6][CH2:7][C:8]2[S:9][CH:10]=[CH:11][C:12]=2[CH2:18]1

参加物

5

反応物 3

HCID 962WaterHCID 7864Chloromethyl Methyl Ether2 回HCID 6454012N-((2-chlorophenyl)methyl)thiophene-3-ethylamine

生成物 1

HCID 65335Ticlopidine Hydrochloride収率 148.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To a solution of 50.8 g (0.2 M) N-(2-chloro-benzyl)-2-(2-thienyl)-ethylamine in 70 ml dimethylformamide heated at 60° C. is added, over 7 minutes, 22.7 g (0.24 M) chloromethylmethylether. The temperature of the reaction medium is maintained at 60° C. throughout the addition step by cooling with water. Thirty minutes after completion of the chloromethylmethylether addition, the medium is cooled to 20° C. The desired product, which has precipitated out, is filtered and washed with 2×70 ml acetone, to give 45.1 g 5-(2-chloro-benzyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine hydrochloride (Yield: 75%).

後処理

  1. additionis added, over 7 minutes
  2. temperaturethe medium is cooled to 20° C
  3. customThe desired product, which has precipitated out
  4. filtrationis filtered
  5. washwashed with 2×70 ml acetone

出典と根拠

ORDレコード
ord-442f27ab40f048bfa75d2aa2a0eb5f7d
出典データセット
uspto-grants-1979_11
特許番号
US04174448

関連ノート

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