Pyridinium chloride → HCID 68554841、化合物

HRID 2359883ノート

反応式

HRID 2359883 の反応式
C[O:2][C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[C:7]1[NH2:16].Cl.N1C=CC=CC=1>O>[NH2:16][C:7]1[N:6]([CH2:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]=2[OH:2])[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1

参加物

4

反応物 2

HCID 10176127Pyridinium chlorideHCID 68550921HCID 68550921、化合物

生成物 1

HCID 68554841HCID 68554841、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

120 mg (0.45 mmol) 3-(2-methoxybenzyl)-3,4-dihydroquinazolin-2-amine and 5 g pyridine hydrochloride were combined and heated for 4 hours at approx. 140° C. After cooling the melt, the residue was dissolved in water, extracted three times with dichloromethane and the combined organic phases were dried, filtered and evaporated. The resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization yielded the target product as a beige white solid; 110 mg.

後処理

  1. temperatureAfter cooling the melt
  2. extractionextracted three times with dichloromethane
  3. customthe combined organic phases were dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization

出典と根拠

ORDレコード
ord-e27a5b14b6bc467db73f5f03f6a8c3b8
出典データセット
uspto-grants-2014_04
特許番号
US08686002B2

反応ノート

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