Ethyl orthoformate → HCID 178468254, 화합물

HRID 1602276노트

반응식

HRID 1602276 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178468254HCID 178468254, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0da026190479461cafee09722ae91152
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05981533

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