Acrylate → HCID 23284684、化合物

HRID 369324ノート

反応式

HRID 369324 の反応式
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([CH3:9])[CH:3]=1.C(O[CH:13]=[C:14]([C:20](=[O:33])[C:21]1[CH:26]=[C:25]([F:27])[C:24]([N+:28]([O-:30])=[O:29])=[C:23]([CH3:31])[C:22]=1F)[C:15]([O:17][CH2:18][CH3:19])=[O:16])C.C([O-])(=O)C=C>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:8]=[CH:7][C:5]([N:6]2[C:22]3[C:21](=[CH:26][C:25]([F:27])=[C:24]([N+:28]([O-:30])=[O:29])[C:23]=3[CH3:31])[C:20](=[O:33])[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13]2)=[C:4]([CH3:9])[CH:3]=1

参加物

5

反応物 3

HCID 25188AcrylateHCID 679824-Fluoro-2-methylanilineHCID 53814737Ethyl α-(ethoxymethylene)-2,5-difluoro-3-methyl-4-nitro-β-oxobenzenepropanoate

生成物 1

HCID 23284684HCID 23284684、化合物収率 46.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of 4-fluoro-2-methylaniline (about 1 g) in chloroform (5 ml) was added dropwise to a solution of ethyl 3-ethoxy-2-(2',5'-difluoro-3'-methyl-4'-nitrobenzoyl)acrylate (2.0 g) in chloroform (10 ml) at room temperature (while confirming the disappearance of the acrylate by tlc). After the mixture was stirred for 10 minutes, the solvent and the like were distilled off. Potassium carbonate (800 mg) was added to a solution of the whole amount of the residue in dimethylformamide (3 ml), and the mixture was stirred at 110° C. for 20 minutes. Chloroform and water were added to the reaction mixture to collect an organic layer. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off. Ethanol was added to the residue to disperse it therein, and filtration was conducted to obtain the title compound (1.1 g) as a pale yellow powder.

後処理

  1. distillationthe solvent and the like were distilled off
  2. additionPotassium carbonate (800 mg) was added to a solution of the whole amount of the residue in dimethylformamide (3 ml)
  3. stirringthe mixture was stirred at 110° C. for 20 minutes
  4. additionChloroform and water were added to the reaction mixture
  5. customto collect an organic layer
  6. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. additionEthanol was added to the residue
  9. additionto disperse it
  10. filtrationfiltration

出典と根拠

ORDレコード
ord-ef0ed69be122427d9eff6823bbde2e42
出典データセット
uspto-grants-2000_10
特許番号
US06136823

反応ノート

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