Water → HCID 22693286、化合物

HRID 1689839ノート

反応式

HRID 1689839 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 22693286HCID 22693286、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-1b21b2602ad049bcad7db8da1035abb4
出典データセット
uspto-grants-2012_04
特許番号
US08153625B2

反応ノート

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