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Cyclobutyl 3-aminocrotonate → Cyclobutyl 5-benzoyl-2,6-dimethyl-4-(2-methyl-4-oxo-4H-chromen-8-yl)-1,4-dihydropyridine-3-carboxylate

HRID 1669765
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HRID 1669765 반응식
[CH3:1][C:2]1[O:3][C:4]2[C:9]([C:10](=[O:12])[CH:11]=1)=[CH:8][CH:7]=[CH:6][C:5]=2[CH:13]=[C:14]([C:23](=O)[CH3:24])[C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:16].[NH2:26]/[C:27](/[CH3:36])=[CH:28]\[C:29]([O:31][CH:32]1[CH2:35][CH2:34][CH2:33]1)=[O:30]>C(O)C>[C:15]([C:14]1[CH:13]([C:5]2[CH:6]=[CH:7][CH:8]=[C:9]3[C:4]=2[O:3][C:2]([CH3:1])=[CH:11][C:10]3=[O:12])[C:28]([C:29]([O:31][CH:32]2[CH2:35][CH2:34][CH2:33]2)=[O:30])=[C:27]([CH3:36])[NH:26][C:23]=1[CH3:24])(=[O:16])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 57475512Cyclobutyl 3-aminocrotonateHCID 673426642-[(2-Methyl-4-oxo-4H-chromen-8-yl)methylene]-1-phenylbutane-1,3-dione

생성물 1

HCID 57503331Cyclobutyl 5-benzoyl-2,6-dimethyl-4-(2-methyl-4-oxo-4H-chromen-8-yl)-1,4-dihydropyridine-3-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

340 mg (1.02 mmol) of 2-[(2-methyl-4-oxo-4H-chromen-8-yl)methylene]-1-phenylbutane-1,3-dione are dissolved with 156 mg (1.8 mmol) of cyclobutyl 3-aminocrotonate in 5 ml of ethanol and heated under reflux under argon for 24 h. The reaction solution is purified by preparative HPLC. Concentration of the product fractions and crystallization from ethyl acetate result in 206 mg (43% of theory) of the title compound as a yellow solid.

후처리

  1. temperatureheated
  2. temperatureunder reflux under argon for 24 h
  3. customThe reaction solution is purified by preparative HPLC
  4. customConcentration of the product fractions and crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-5bfe87ba3bac4c1da4a2adfdb34b731d
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989633B2

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