Ethyl orthoformate → HCID 178468254、化合物

HRID 1602276ノート

反応式

HRID 1602276 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=2)[C:3]=1[C:16]#[N:17].[CH2:18]([O:20][CH:21](OCC)OCC)[CH3:19]>C(O)C>[C:16]([C:3]1[C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=2)=[N:5][NH:6][C:2]=1[N:1]=[CH:21][O:20][CH2:18][CH3:19])#[N:17]

参加物

4

反応物 2

HCID 31214Ethyl orthoformateHCID 107280981H-Pyrazole-4-carbonitrile, 3-amino-5-[(3-methoxyphenyl)amino]-

生成物 1

HCID 178468254HCID 178468254、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
120 °C

実験手順

With stirring, a mixture of 4 g (17.45 mmol) of 5-amino-4-cyano-3-(3-methoxy-phenylamino)-pyrazole (Step 50.1) and 50 ml of orthoformic acid triethyl ester is heated at 120° C. for 1.5 hours, care being taken to ensure that the ethanol formed in the course of the reaction is distilled off from the reaction mixture. The reaction mixture is cooled to 30° C., approx. 100 ml of diethyl ether are added and the reaction mixture is cooled further to 0° C. and filtered. Washing with diethyl ether yields the title compound; m.p. 181-183° C.

後処理

  1. customformed in the course of the reaction
  2. distillationis distilled off from the reaction mixture
  3. temperatureThe reaction mixture is cooled to 30° C.
  4. additionapprox. 100 ml of diethyl ether are added
  5. temperaturethe reaction mixture is cooled further to 0° C.
  6. filtrationfiltered
  7. washWashing with diethyl ether

出典と根拠

ORDレコード
ord-0da026190479461cafee09722ae91152
出典データセット
uspto-grants-1999_11
特許番号
US05981533

反応ノート

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