Ethyl Acetate → HCID 13302197、化合物

HRID 1903720ノート

反応式

HRID 1903720 の反応式
[CH2:1]([O:3][C:4]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[O:24][CH3:25])[CH2:14][CH2:13]1)=[O:5])[CH3:2].C(OCC)(=O)C.[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]/[C:35]([OH:37])=[O:36]>C(O)C>[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]/[C:35]([OH:37])=[O:36].[CH2:1]([O:3][C:4]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[O:24][CH3:25])[CH2:14][CH2:13]1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 133623Sgb 483HCID 444972Fumaric Acid

生成物 1

HCID 13302197HCID 13302197、化合物収率 79.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 3.48 g (0.01 mol) of the 1-(6-ethoxycarbonylhexyl)-4-(o-methoxyphenyl)piperazine in 50 ml of a mixture of ethyl acetate and ethanol (vol. ratio=50:1) was stirred with 1.16 g (0.01 mol) of fumaric acid at 60° C. for 30 minutes. The mixture was left to stand overnight under cooling to give 3.71 g of 1-(6-ethoxycarbonylhexyl)-4-(o-methoxyphenyl)piperazine fumarate. The fumarate was recrystallized from a mixture of ethyl acetate and ethanol (vol. ratio=50:1) to give an analytically pure fumarate having a melting point of 101°-102° C.

後処理

  1. waitThe mixture was left
  2. temperatureunder cooling

出典と根拠

ORDレコード
ord-b6a864158e134df689edf95fd9039d75
出典データセット
uspto-grants-1984_03
特許番号
US04438115

反応ノート

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