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Dichloromethane → 4-(3-Hydroxy-4-methylanilino)-6-methoxy-7-(4-pyridylmethoxy)quinazoline hydrochloride

HRID 279494
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HRID 279494 반응식
C([O:4][C:5]1[CH:6]=[C:7]([CH:29]=[CH:30][C:31]=1[CH3:32])[NH:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=3)=[C:16]([O:19][CH3:20])[CH:17]=2)[N:12]=[CH:11][N:10]=1)(=O)C.[OH-].[Na+].C(Cl)[Cl:36]>CO>[ClH:36].[OH:4][C:5]1[CH:6]=[C:7]([CH:29]=[CH:30][C:31]=1[CH3:32])[NH:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=3)=[C:16]([O:19][CH3:20])[CH:17]=2)[N:12]=[CH:11][N:10]=1
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참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 110373874-(3-Acetoxy-4-methylanilino)-6-methoxy-7-(4-pyridylmethoxy)quinazoline

생성물 1

HCID 226249114-(3-Hydroxy-4-methylanilino)-6-methoxy-7-(4-pyridylmethoxy)quinazoline hydrochloride수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4-(3-acetoxy-4-methylanilino)-6-methoxy-7-(4-pyridylmethoxy)quinazoline (93 mg, 0.2 mmol) in a mixture of methanol (6 ml) and methylene chloride (3 ml) was added at ambient temperature a 2M aqueous sodium hydroxide solution (0.3 ml, 0.6 mmol). The mixture was stirred for 10 minutes at ambient temperature, the solvents were partially evaporated, water was added to the residue and the solution was acidified with 0.1M hydrochloric acid to pH6. The precipitate was filtered off, washed with water and dried under vacuum to give 4-(3-hydroxy-4-methylanilino)-6-methoxy-7-(4-pyridylmethoxy)quinazoline hydrochloride (67 mg, 87%).

후처리

  1. customthe solvents were partially evaporated
  2. additionwater was added to the residue
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-cd11878dd20942aabbc9cb64e1d4a0c0
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06362336B1

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