Triethylamine → HCID 21276268, 화합물

HRID 476692노트

반응식

HRID 476692 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:22])[CH2:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(N(CC)CC)C.ClC(OCC)=O.[C:36]1([NH:42][CH2:43][CH2:44][NH2:45])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:22])[CH2:15][CH2:16][CH2:17][CH2:18][C:19]([NH:45][CH2:44][CH2:43][NH:42][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[O:21])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 742701,2-Ethanediamine, N1-phenyl-HCID 139357676-[2-(3,4-Dimethoxyphenyl)ethylamino]-6-oxohexanoic acid

생성물 1

HCID 21276268HCID 21276268, 화합물수율 65.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

6-[2-(3,4-Dimethoxyphenyl)ethylamino]-6-oxohexanoic acid (6.0 g, 0.19) was dissolved in dry dichloromethane (200 ml) and triethylamine (2.28 g, 0.021 mole), and ethyl chloroformate (1.86 ml, 0.019 mole) added at O°. After 1 hour at 0° N-phenyl-1,2-ethanediamine (2.64 g, 0.019 mole) was added and the mixture stirred at room temperature for 18 hr. After washing with water and drying (Na2SO4), the reaction mixture was evaporated and the residue recrystallised from ethyl acetate to give the sub title compound (5.3 g) mp 109°-11°.

후처리

  1. washAfter washing with water
  2. dry with materialdrying (Na2SO4)
  3. customthe reaction mixture was evaporated
  4. customthe residue recrystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-5ac0513627c849a08a59ec480418c9bd
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04885313

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