HCID 10976898, 화합물 → HCID 20277264, 화합물

HRID 1164649노트

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HRID 1164649 반응식
[C:1]([C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH:5]=[C:6]([C:13]([CH3:15])=O)[C:7]([O:9]CCCl)=[O:8])#[N:2].[NH2:20]/[C:21](/[CH:28]([O:32][CH2:33][CH3:34])[O:29][CH2:30][CH3:31])=[CH:22]\[C:23]([O:25][CH2:26][CH3:27])=[O:24]>C(OCC)(=O)C>[C:1]([C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH:5]1[C:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[C:21]([CH:28]([O:32][CH2:33][CH3:34])[O:29][CH2:30][CH3:31])[NH:20][C:13]([CH3:15])=[C:6]1[C:7]([OH:9])=[O:8])#[N:2]

참가 물질

4

반응물 2

HCID 10976898HCID 10976898, 화합물HCID 543701612-Chloroethyl 2-(2-cyanobenzylidene)acetoacetate

생성물 1

HCID 20277264HCID 20277264, 화합물수율 82.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2-chloroethyl 2-(2-cyanobenzylidene)acetoacetate (4.72 g) and ethyl 3-amino-4,4-diethoxycrotonate (4.06 g) was heated for 3 hours at 100°~105° C. with stirring. After cooling, the reaction mixture was dissolved in ethyl acetate, and the solution was washed twice with an aqueous solution of sodium chloride and then dried over magnesium sulfate. After removal of the solvent under reduced pressure, the residual oil was chromatographed over silica gel with a mixture of benzene and ethyl acetate (5:1 V/V) to give 2-chloroethyl ester of 4-(2-cyanophenyl)-5-ethoxycarbonyl-6-diethoxymethyl-2-methyl-1,4-dihydropyridine-3-carboxylic acid (5.81 g).

후처리

  1. temperaturewas heated for 3 hours at 100°~105° C.
  2. temperatureAfter cooling
  3. washthe solution was washed twice with an aqueous solution of sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. customAfter removal of the solvent under reduced pressure
  6. customthe residual oil was chromatographed over silica gel with a mixture of benzene and ethyl acetate (5:1 V/V)

출처 및 근거

ORD 기록
ord-36ace416209d4731b33efcb5f9c609b9
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04370334

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