HCID 10976898、化合物 → HCID 20277264、化合物

HRID 894725ノート

反応式

HRID 894725 の反応式
[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]

参加物

4

反応物 2

HCID 10976898HCID 10976898、化合物HCID 543701612-Chloroethyl 2-(2-cyanobenzylidene)acetoacetate

生成物 1

HCID 20277264HCID 20277264、化合物収率 82.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-98d06d6d4bc74f4ab531df5ee852eaa6
出典データセット
uspto-grants-1981_08
特許番号
US04284634

反応ノート

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