Diethylethanolamine → HCID 69413793、化合物

HRID 1371563

反応式

HRID 1371563 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].[CH3:12]CN(CCO)CC.BrC[C:22]([NH:24][C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([F:34])([F:33])[F:32])[CH:26]=1)=[O:23]>ClCCl>[F:32][C:31]([F:33])([F:34])[C:27]1[CH:26]=[C:25]([NH:24][C:22]([N:1]([CH3:12])[CH2:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:8])([CH3:10])[CH3:9])=[O:23])[CH:30]=[CH:29][CH:28]=1

参加物

5

反応物 3

HCID 7497DiethylethanolamineHCID 187201N-BOC-ethylenediamineHCID 23171522-bromo-N-[3-(trifluoromethyl)phenyl]acetamide

生成物 1

HCID 69413793HCID 69413793、化合物収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Tert-butyl 2-aminoethylcarbamate (0.32 g, 2 mmol) was dissolved in dichloromethane with DEEA (0.6 mL, 3.4 mmol). To this solution, 2-bromo-N-(3-(trifluoromethyl)-phenyl)acetamide was added and the reaction mixture stirred for 6 hours at room temperature. The reaction mixture was concentrated to an oil and purified by column chromatography (eluent: EtOAC) to give the product 0.37 g, 1.02 mmol, 50% yield. 1H NMR (500 MHz, CDCl3) δ 9.39 (s, 1H), 7.82 (s, 1H), 7.78 (d, J=7.8 Hz, 1H), 7.37 (t, J=7.9 Hz, 1H), 7.28 (d, J=7.8 Hz, 1H), 4.68 (s, 1H), 3.36 (s, 2H), 3.22 (dd, J=11.2, 5.5 Hz, 2H), 2.74 (t, J=5.7 Hz, 2H).

後処理

  1. concentrationThe reaction mixture was concentrated to an oil
  2. custompurified by column chromatography (eluent: EtOAC)

出典と根拠

ORDレコード
ord-b0dd1572082e4c9399bb4781fde2f6af
出典データセット
uspto-grants-2007_01
特許番号
US07157476B2

関連ノート

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