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5-Amino-4-fluoro-2-methylphenol → ZM 323881 hydrochloride

HRID 1737595
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HRID 1737595 반응식
[F:1][C:2]1[CH:8]=[C:7]([CH3:9])[C:6]([OH:10])=[CH:5][C:3]=1[NH2:4].Cl.[CH2:12]([O:19][C:20]1[CH:29]=[C:28]2[C:23]([C:24]([Cl:30])=[N:25][CH:26]=[N:27]2)=[CH:22][CH:21]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CC(O)CCC>[ClH:30].[CH2:12]([O:19][C:20]1[CH:29]=[C:28]2[C:23]([C:24]([NH:4][C:3]3[CH:5]=[C:6]([OH:10])[C:7]([CH3:9])=[CH:8][C:2]=3[F:1])=[N:25][CH:26]=[N:27]2)=[CH:22][CH:21]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 101540985-Amino-4-fluoro-2-methylphenolHCID 226250837-Benzyloxy4-chloroquinazoline hydrochloride

생성물 1

HCID 22624897ZM 323881 hydrochloride수율 80.4%

시약·촉매·용매 1

HCID 223862-Pentanol용매

반응 조건

온도
120 °C

실험 절차

2-Fluoro-5-hydroxy-4-methylaniline (170 mg, 1.2 mmol), (prepared as described for the starting material in Example 13), was added to a solution of 7-benzyloxy-4-chloroquinazoline hydrochloride (307 mg, 1 mmol) in 2-pentanol (5 ml) and the mixture stirred at 120° C. for 2 hours. The mixture was allowed to cool and the resulting precipitate was collected by filtration, washed with isopropanol and then ether and dried under vacuum at 70° C. to give 7-benzyloxy-4-(2-fluoro-5-hydroxy-4-methylanilino)quinazoline hydrochloride (331 mg, 80%).

후처리

  1. temperatureto cool
  2. filtrationthe resulting precipitate was collected by filtration
  3. washwashed with isopropanol
  4. dry with materialether and dried under vacuum at 70° C.

출처 및 근거

ORD 기록
ord-26202637ea2b402884c682ab403cef48
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05962458

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