Furfurylamine → HCID 9291888、化合物

HRID 1022395ノート

反応式

HRID 1022395 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.[CH2:19]([NH2:25])[C:20]1[O:24][CH:23]=[CH:22][CH:21]=1>O>[Cl:18][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([NH:25][CH2:19][C:20]1[O:24][CH:23]=[CH:22][CH:21]=1)[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 3438FurfurylamineHCID 16282212,6-dichloro-4-phenylquinazoline

生成物 1

HCID 9291888HCID 9291888、化合物収率 83.4%

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 486 mg of furfurylamine was stirred at 85° C. for 40 minutes and then poured into 50 ml of water. The mixture was extracted with ethyl acetate and the resultant extract was washed with water and then concentrated. The resulting residue was recrystallized from ethanol to obtain 280 mg of the titled compound. Mp.142.0° C. 1H NMR (CDCl3): 4.77 (2H, d, J=5.6 Hz), 5.70 (1H, br. t, J=5.6 Hz), 6.29-6.32 (2H, m), 7.36 (1H, dd, J=1.8, 0.9 Hz), 7.53-7.70 (7H, m), 7.78 (1H, d, J=2.2 Hz).

後処理

  1. extractionThe mixture was extracted with ethyl acetate
  2. extractionthe resultant extract
  3. washwas washed with water
  4. concentrationconcentrated
  5. customThe resulting residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-a2dd70be6ab64e4b877cb80455e4458e
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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