Methylhydrazine → HCID 13949475, 화합물

HRID 1022400노트

반응식

HRID 1022400 반응식
Cl[C:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:18])[CH:8]=2)[N:3]=1.[CH3:19][NH:20][NH2:21]>O>[Cl:18][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([N:20]([CH3:19])[NH2:21])[N:11]=[C:10]2[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 16282212,6-dichloro-4-phenylquinazoline

생성물 1

HCID 13949475HCID 13949475, 화합물수율 79.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 275 mg of 2,6-dichloro-4-phenylquinazoline (compound No. Ia1-3) and 461 mg of monomethylhydrazine was stirred at 85° C. for 30 minutes. The resulting reaction product was cooled and 200 ml of water was added thereto. Precipitated crystals were collected by filtration and the collected product was purified by column chromatography (ethyl acetate) to obtain 225 mg of the titled compound. Mp. 155.9° C. 1H NMR (CDCl3): 3.52 (3H, s), 4.65 (2H, s), 7.54-7.63 (5H, m), 7.70-7.74 (2H, m), 7.80 (1H, d, J=2.0 Hz).

후처리

  1. customThe resulting reaction product
  2. temperaturewas cooled
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration
  5. customthe collected product was purified by column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-ebfde4168a804d758631345bd0eec041
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722580B2

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