Water → HCID 22693286, 화합물

HRID 1689839노트

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HRID 1689839 반응식
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(N(CC)CC)C.[NH:20]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.O>O1CCCC1>[Cl:1][C:2]1[N:11]=[C:10]([N:20]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8119AzepaneHCID 8471TriethylamineHCID 2528862,4-Dichloroquinazoline

생성물 1

HCID 22693286HCID 22693286, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2,4-dichloroquinazoline (1.0 g) in tetrahydrofuran (10 mL) were added triethylamine (2.1 mL) and perhydroazepine (0.745 mL) with ice cooling and the mixture was stirred for 1 hour at room temperature. To the reaction mixture was added water (20 mL) and the resulting mixture was concentrated. The residue was extracted with methylene chloride three times. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was washed with hexane-diethyl ether (10:1) to give the title compound (991 mg) having the following physical data.

후처리

  1. concentrationthe resulting mixture was concentrated
  2. extractionThe residue was extracted with methylene chloride three times
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. washThe residue was washed with hexane-diethyl ether (10:1)

출처 및 근거

ORD 기록
ord-1b21b2602ad049bcad7db8da1035abb4
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153625B2

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