Diethylamine → Methyl 3-(2-ethoxycarbonylvinyl)-5-(3,4,5-trifluorophenyl)piperazine-1-carboxylate

HRID 554006ノート

反応式

HRID 554006 の反応式
C(NCC)C.[CH3:6][O:7][C:8]([N:10]1[CH2:15][CH:14]([C:16]2[CH:21]=[C:20]([F:22])[C:19]([F:23])=[C:18]([F:24])[CH:17]=2)[N:13](C(OCC2C3C=CC=CC=3C3C2=CC=CC=3)=O)[CH:12]([CH:42]=[CH:43][C:44]([O:46][CH2:47][CH3:48])=[O:45])[CH2:11]1)=[O:9]>C(#N)C>[CH2:47]([O:46][C:44]([CH:43]=[CH:42][CH:12]1[NH:13][CH:14]([C:16]2[CH:21]=[C:20]([F:22])[C:19]([F:23])=[C:18]([F:24])[CH:17]=2)[CH2:15][N:10]([C:8]([O:7][CH3:6])=[O:9])[CH2:11]1)=[O:45])[CH3:48]

参加物

4

反応物 2

HCID 8021DiethylamineHCID 67460768HCID 67460768、化合物

生成物 1

HCID 67464101Methyl 3-(2-ethoxycarbonylvinyl)-5-(3,4,5-trifluorophenyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Diethylamine (2 mL) was added to a solution of 2-(2-ethoxycarbonylvinyl)-6-(3,4,5-trifluorophenyl)piperazine-1,4-dicarboxylic acid 1-(9H-fluoren-9-ylmethyl) ester 4-methyl ester (1.03 g) in acetonitrile (10 mL), and the reaction solution was stirred at room temperature for one hour. The reaction solution was concentrated, and the residue was purified by silica gel column chromatography (heptane->ethyl acetate) to obtain 422 mg of an E/Z isomer mixture of the title compound. The property value of the compound is as follows.

後処理

  1. concentrationThe reaction solution was concentrated
  2. customthe residue was purified by silica gel column chromatography (heptane->ethyl acetate)
  3. customto obtain

出典と根拠

ORDレコード
ord-0fe97f69f1be4f8493f5484152280e3d
出典データセット
uspto-grants-2011_11
特許番号
US08048878B2

反応ノート

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