1-Chloroethyl chloroformate → 1-(Benzothiophen-2-yl)piperazine hydrochloride

HRID 1900560ノート

反応式

HRID 1900560 の反応式
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[S:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[CH:18]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:23]C(OC(Cl)=O)C>ClCCl>[ClH:23].[S:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[CH:18]=[C:14]1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 217016231-Benzyl-4-(benzothiophen-2-yl)piperazine

生成物 1

HCID 190649731-(Benzothiophen-2-yl)piperazine hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-benzyl-4-(benzothiophen-2-yl)piperazine (1.5 g, 4.9 mmol) in anhydrous dichloromethane (20 ml) at 0° C. under nitrogen was added 1-chloroethylchloroformate (0.68 ml, 6.37 mmol). The mixture was allowed to warm to room temperature, stirred for 1 h and concentrated in vacuo. The crude residue was dissolved in methanol (10 ml) and heated to reflux for 30 minutes, left to cool and the title compound collected by filtration (0.6 g), m.p. 240° C. (dec.).

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe crude residue was dissolved in methanol (10 ml)
  3. temperatureheated
  4. temperatureto reflux for 30 minutes
  5. waitleft
  6. temperatureto cool
  7. filtrationthe title compound collected by filtration (0.6 g), m.p. 240° C. (dec.)

出典と根拠

ORDレコード
ord-67a08c733cb949368f22a3192202c0ff
出典データセット
uspto-grants-1996_11
特許番号
US05576319

反応ノート

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