Ammonia → 6-Methoxy-7-(3-(4-methylpiperazin-1-yl)propoxy)-3,4-dihydroquinazolin-4-one

HRID 454238노트

반응식

HRID 454238 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:30])[N:17](COC(=O)C(C)(C)C)[CH:18]=[N:19]3)=[CH:14][C:13]=2[O:31][CH3:32])[CH2:4][CH2:3]1.N>CO>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:30])[NH:17][CH:18]=[N:19]3)=[CH:14][C:13]=2[O:31][CH3:32])[CH2:6][CH2:7]1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 220306066-Methoxy-7-(3-(4-methylpiperazin-1-yl)propoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one

생성물 1

HCID 1354581696-Methoxy-7-(3-(4-methylpiperazin-1-yl)propoxy)-3,4-dihydroquinazolin-4-one수율 95.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 7-(3-(4-methylpiperazin-1-yl)propoxy)-6-methoxy-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (31.8 g, 71.3 mmol) in methanol saturated with ammonia was stirred at ambient temperature overnight. The volatiles were removed under vacuum. The solid was triturated with ether containing about 10% of methylene chloride, filtered, washed with ether containing about 10% methylene chloride and dried under vacuum to give 7-(3-(4-methylpiperazin-1-yl)propoxy)-6-methoxy-3,4-dihydroquinazolin-4-one (22.63 g, 95%).

후처리

  1. customThe volatiles were removed under vacuum
  2. customThe solid was triturated with ether containing about 10% of methylene chloride
  3. filtrationfiltered
  4. washwashed with ether containing about 10% methylene chloride
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-fbdd7638d0f6465d8bbe59ea90241b24
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492560B2

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