Diketene → Butanoic acid, 3-oxo-, 2-[4-(diphenylmethyl)-1-piperazinyl]ethyl ester

HRID 329882

反応式

HRID 329882 の反応式
[CH:1]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][OH:22])[CH2:16][CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:23]=[C:24]1[O:28][C:26](=[O:27])[CH2:25]1>>[C:26]([O:22][CH2:21][CH2:20][N:17]1[CH2:16][CH2:15][N:14]([CH:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:19][CH2:18]1)(=[O:27])[CH2:25][C:24]([CH3:23])=[O:28]

参加物

3

反応物 2

HCID 12661DiketeneHCID 47425734-(Diphenylmethyl)-1-piperazineethanol

生成物 1

HCID 11740518Butanoic acid, 3-oxo-, 2-[4-(diphenylmethyl)-1-piperazinyl]ethyl ester

実験手順

To 4-benzhydryl-1-piperazineethanol (18.1 g) was added diketene (5.1 g) and the mixture was heated under stirring at 70°-80° C. for 1.5 hours. The product obtained was purified by silica gel chromatography [eluent: hexaneethyl acetate (3:2)] to give 2-(4-benzhydryl-1-piperazinyl)-ethyl acetoacetate as an oil. Yield 17.1 g (73.6%). IR(Neat): 1730, 1715 cm-1. NMR(CDCl3)δ: 2.22(3H, s), 2.43(10H, broad) 3.39(2H, s), 4.18(1H, s), 4.20(2H, t, J=6), 6.64-7.73(10H, m).

後処理

  1. temperaturethe mixture was heated
  2. customThe product obtained
  3. customwas purified by silica gel chromatography [eluent: hexaneethyl acetate (3:2)]

出典と根拠

ORDレコード
ord-63ebb8209b674891a7f623bcd75b5092
出典データセット
uspto-grants-1990_01
特許番号
US04892875

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