Triethylamine → t-Butyl 4-(4-methoxycarbonylbenzoyl)piperazine-1-carboxylate

HRID 747682ノート

反応式

HRID 747682 の反応式
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl-].[C:22]([O:33][CH3:34])(=[O:32])[C:23]1[CH:31]=[CH:30][C:26]([C:27]([O-])=[O:28])=[CH:25][CH:24]=1>CN(C)C=O.Cl>[CH3:34][O:33][C:22]([C:23]1[CH:31]=[CH:30][C:26]([C:27]([N:4]2[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]2)=[O:28])=[CH:25][CH:24]=1)=[O:32]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 22493623Monomethyl terephthalate chloride

生成物 1

HCID 17789205t-Butyl 4-(4-methoxycarbonylbenzoyl)piperazine-1-carboxylate

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒

実験手順

4.93 g (26.5 mmol) of t-butyl piperazine-1-carboxylate and 4.8 ml (34.5 mmol) of triethylamine were stirred in 50 ml of dimethylformamide under cooling with ice. 5.25 g (26.5 mmol) of monomethyl terephthalate chloride was slowly added to the resultant mixture, and they were stirred for 16 hours. The temperature was elevated to room temperature, and the reaction liquid was diluted with 1 N hydrochloric acid. After the extraction with ethyl acetate followed by the treatment in an ordinary manner, the title compound was obtained.

後処理

  1. temperatureunder cooling with ice
  2. customwas elevated to room temperature
  3. customthe reaction liquid
  4. extractionAfter the extraction with ethyl acetate

出典と根拠

ORDレコード
ord-f920af3f16aa4415b543e2effaf1a3a1
出典データセット
uspto-grants-2008_07
特許番号
US07396844B1

反応ノート

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