Methylhydrazine → HCID 13949475、化合物

HRID 1022400ノート

反応式

HRID 1022400 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 13949475HCID 13949475、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ebfde4168a804d758631345bd0eec041
出典データセット
uspto-grants-2014_05
特許番号
US08722580B2

反応ノート

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