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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Butenoic acid, 3-amino-, 1-methylethyl ester → 4-(2-Cyanophenyl)-5-methoxycarbonyl-6-dimethoxymethyl-2-methyl-1,4-dihydropyridine-3-carboxylic acid

HRID 1759117
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HRID 1759117 반응식
[C:1]([C:3]1[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=1[CH:5]=[C:6]([C:11]([CH:13]([O:16][CH3:17])[O:14][CH3:15])=O)[C:7]([O:9][CH3:10])=[O:8])#[N:2].[NH2:22]/[C:23](/[CH3:31])=[CH:24]\[C:25]([O:27]C(C)C)=[O:26]>C(OCC)(=O)C>[C:1]([C:3]1[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=1[CH:5]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[C:11]([CH:13]([O:16][CH3:17])[O:14][CH3:15])[NH:22][C:23]([CH3:31])=[C:24]1[C:25]([OH:27])=[O:26])#[N:2]
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참가 물질

4

반응물 2

HCID 111372742-Butenoic acid, 3-amino-, 1-methylethyl esterHCID 53675930Methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate

생성물 1

HCID 202772614-(2-Cyanophenyl)-5-methoxycarbonyl-6-dimethoxymethyl-2-methyl-1,4-dihydropyridine-3-carboxylic acid수율 68.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate (10.1 g) and isopropyl 3-aminocrotonate (5.51 g) was heated for 40 minutes at 78° C. and for 5.5 hours at 120° C. with stirring, followed by heating for an hour at 125° C. without the stirring. After the reaction mixture was allowed to stand overnight, it was dissolved in ethyl acetate. This solution was washed twice with water, dried and then evaporated to dryness under reduced pressure to give a residue, which was crystallized from ethyl ether. The crystals were collected by filtration and washed with a small amount of ethyl ether to give crude powder of isopropyl ester of 4-(2-cyanophenyl)-5-methoxycarbonyl-6-dimethoxymethyl-2-methyl-1,4-dihydropyridine-3-carboxylic acid (8.96 g). Further, the crude product (0.77 g) was recovered from the filtrate. 0.5 g Of this crude product was recrystallized from isopropyl ether to give purified white powder of the same product (0.37 g), mp 171°-172.5° C.

후처리

  1. temperatureby heating for an hour at 125° C. without the stirring
  2. washThis solution was washed twice with water
  3. customdried
  4. customevaporated to dryness under reduced pressure
  5. customto give a residue, which
  6. customwas crystallized from ethyl ether
  7. filtrationThe crystals were collected by filtration
  8. washwashed with a small amount of ethyl ether

출처 및 근거

ORD 기록
ord-8a4ac1fec8f944118eefef6809d832b7
출처 데이터셋
uspto-grants-1982_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04338322

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