Methanol → HCID 18796796, 화합물

HRID 2392880노트

반응식

HRID 2392880 반응식
B(Cl)(Cl)[Cl:2].C1[O:26][C:25]2[CH:24]=[CH:23][C:9]([CH2:10][NH:11][C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([Cl:22])[CH:20]=4)[N:15]=[CH:14][N:13]=3)=[CH:8][C:7]=2[O:6]1.CO>C(Cl)Cl.C(Cl)(Cl)Cl>[ClH:2].[OH:6][C:7]1[CH:8]=[C:9]([CH:23]=[CH:24][C:25]=1[OH:26])[CH2:10][NH:11][C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([Cl:22])[CH:20]=2)[N:15]=[CH:14][N:13]=1

참가 물질

6

반응물 3

HCID 887MethanolHCID 25135Boron TrichlorideHCID 6610310N-(1,3-benzodioxol-5-ylmethyl)-6-chloroquinazolin-4-amine

생성물 1

HCID 18796796HCID 18796796, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

40 ml of a 1.0M solution of boron trichloride in methylene chloride was dropped into a solution of 2.00 g (6.37 mmol) of 4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline in 150 ml of chloroform under stirring at room temperature. The obtained mixture was stirred at room temperature for 2 days, followed by the addition of methanol, and the obtained mixture was distilled under a reduced pressure to remove the solvent. This procedure was repeated twice. The crystals thus precipitated were washed with methanol and recrystallized from ethanol to give 1.53 g of the title compound as a yellow crystal.

후처리

  1. stirringThe obtained mixture was stirred at room temperature for 2 days
  2. distillationthe obtained mixture was distilled under a reduced pressure
  3. customto remove the solvent
  4. customThe crystals thus precipitated
  5. washwere washed with methanol
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-cba0d1ed2f994ace9d8d0fd1841bc66b
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05801180

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