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

HRID 617182

반응식

HRID 617182 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-91c7730f43df421a9a14133717031f4a
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05948786

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