2-Chloroethyl formate → 1-Ethoxycarbonyl-4-ethoxycarbonyl-mercapto-piperidine

HRID 236334

反応式

HRID 236334 の反応式
Cl[CH2:2][CH2:3][O:4][CH:5]=[O:6].C[N:8]1[CH2:13][CH2:12][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10][CH:9]1[SH:19]>C1(C)C=CC=CC=1>[CH2:3]([O:4][C:5]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10][CH:9]1[SH:19])=[O:6])[CH3:2]

参加物

4

反応物 2

HCID 2467482-Chloroethyl formate2 回HCID 198133811-Methyl-4-ethoxycarbonyl-mercapto-piperidine

生成物 1

HCID 202169741-Ethoxycarbonyl-4-ethoxycarbonyl-mercapto-piperidine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

106.3 g (0.88 mol) of chloroethylformate are added dropwise with stirring over a period of 30 minutes to a solution of 100 g (0.48 mol) of 1-methyl-4-ethoxycarbonyl-mercapto-piperidine in 80 ml of toluene which has been heated to 90° C. The solution is then heated for two hours to from 100° to 110° C. After repeated addition of 40 g of chloroethylformate the solution is heated for a further three hours. After leaving it to stand overnight at room temperature it is drawn off by suction using a glass fibre filter. The solution is concentrated on a rotary evaporator and the residue is distilled off. 20 g (94% of the theoretical yield) of 1-ethoxycarbonyl-4-ethoxycarbonyl-mercapto-piperidine are obtained. B.P. 138°-140° C.

後処理

  1. temperatureThe solution is then heated for two hours to from 100° to 110° C
  2. temperatureis heated for a further three hours
  3. customAfter leaving it
  4. concentrationThe solution is concentrated on a rotary evaporator
  5. distillationthe residue is distilled off

出典と根拠

ORDレコード
ord-1a343854b68b4651b8f9da0712b06283
出典データセット
uspto-grants-1987_02
特許番号
US04643995

関連ノート

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