Methyl vinyl ketone → 4-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)piperidino]-2-butanone

HRID 616224

反応式

HRID 616224 の反応式
[CH3:1][C:2]([CH:4]=[CH2:5])=[O:3].[CH:6]1[C:16]2[C:15](=[C:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[C:14]3[CH:23]=[CH:24][CH:25]=[CH:26][C:13]=3[CH2:12][S:11][C:10]=2[CH:9]=[CH:8][CH:7]=1.C([O-])(=O)/C=C/C([O-])=O.C1C2C(=C3CCN(C)CC3)C3C=CC=CC=3CSC=2C=CC=1>C(O)C>[CH:6]1[C:16]2[C:15](=[C:17]3[CH2:22][CH2:21][N:20]([CH2:5][CH2:4][C:2](=[O:3])[CH3:1])[CH2:19][CH2:18]3)[C:14]3[CH:23]=[CH:24][CH:25]=[CH:26][C:13]=3[CH2:12][S:11][C:10]=2[CH:9]=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 6570Methyl vinyl ketoneHCID 121108Piperidine, 4-(dibenzo(b,e)thiepin-6(11H)-ylidene)-1-methyl-, hydrochlorideHCID 5460307FumarateHCID 150779404-dibenzo[b,e]thiepin-11(6H)-ylidenepiperidine

生成物 1

HCID 203714844-[4-(6,11-Dihydrodibenzo[b,e]thiepin-11-ylidene)piperidino]-2-butanone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 2.8 g of methylvinylketone in 5 cc of ethanol is added dropwise within 2 minutes to a solution of 7.8 g of 4-(6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)piperidine [M.P. of the fumarate 245°-247°, produced in a manner analogous to that described in Example 9(a), from 4-(6,11-dihydrodibenzo[b,e]thiepin-11-ylidene)-1-methylpiperidine] in 25 cc of ethanol. The reaction mixture is heated at reflux for 1 hour, is then completely concentrated at reduced pressure, and the oily residue, the title compound, is converted into the hydrogen fumarate form. M.P. 180°-182° (decomp.) from ethanol.

後処理

  1. customproduced in a manner analogous to
  2. temperatureThe reaction mixture is heated
  3. temperatureat reflux for 1 hour
  4. concentrationis then completely concentrated at reduced pressure

出典と根拠

ORDレコード
ord-1bf072ad69b042298bd4f8781556ed18
出典データセット
uspto-grants-1978_02
特許番号
US04072756

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