Phenyl isocyanate → 2-Amino-4-(1-phenylcarbamoyl-4-piperidinyl)quinazoline

HRID 617182

反応式

HRID 617182 の反応式
[NH2:1][C:2]1[N:11]=[C:10]([CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(N(CC)CC)C.[C:25]1([N:31]=[C:32]=[O:33])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>ClCCl>[NH2:1][C:2]1[N:11]=[C:10]([CH:12]2[CH2:17][CH2:16][N:15]([C:32](=[O:33])[NH:31][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

5

反応物 3

HCID 7672Phenyl isocyanateHCID 8471TriethylamineHCID 154287752-Amino-4-(4-piperidinyl)quinazoline

生成物 1

HCID 218515192-Amino-4-(1-phenylcarbamoyl-4-piperidinyl)quinazoline収率 87%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-amino-4-(4-piperidinyl)quinazoline (100 mg, 0.44 mmol) obtained in Example 11(1) and triethylamine (133 mg, 1.3 mmol) in dichloromethane (50 ml) was added phenyl isocyanate (50 mg, 0.42 mmol) under a nitrogen atmosphere. The mixture was stirred for about 3 hours at room temperature. The reaction mixture was washed with saturated sodium hydrogencarbonate aqueous solution. The organic layer was dried over sodium sulfate and evaporated in vacuo. The residue was purified by silicagel column chromatography (chloroform:methanol=99:1) to give the titled compound (127 mg).

後処理

  1. washThe reaction mixture was washed with saturated sodium hydrogencarbonate aqueous solution
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customevaporated in vacuo
  4. customThe residue was purified by silicagel column chromatography (chloroform:methanol=99:1)

出典と根拠

ORDレコード
ord-91c7730f43df421a9a14133717031f4a
出典データセット
uspto-grants-1999_09
特許番号
US05948786

関連ノート

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