Triethylamine → HCID 19392157、化合物

HRID 1648219

反応式

HRID 1648219 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.[CH3:20][C:21]([NH2:26])([CH3:25])[CH2:22][O:23][CH3:24]>>[CH3:20][C:21]([NH:26][C:10]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]([Cl:1])[N:11]=1)([CH3:25])[CH2:22][O:23][CH3:24]

参加物

4

反応物 3

HCID 8471TriethylamineHCID 886661-Methoxy-2-methylpropan-2-amineHCID 2528862,4-Dichloroquinazoline

生成物 1

HCID 19392157HCID 19392157、化合物収率 13.2%

実験手順

A mixture of 2,4-dichloroquinazoline (995 mg, 5 mmol), triethylamine (0.7 ml, 5 mmol) and 1,1-dimethyl-2-methoxyethylamine (30 mL, 0.5M methanol sol., 15 mmol) was stood at room temperature for 1 week. The reaction mixture was concentrated and partitioned between ethyl acetate and water. Organic layer was washed with water and brine, dried over MgSO4 and concentrated. The residue was purified on 50 g of silica gel column eluting with 50% ethyl acetate in hexane to obtain the title compound (176 mg) as a white solid.

後処理

  1. waitwas stood at room temperature for 1 week
  2. concentrationThe reaction mixture was concentrated
  3. custompartitioned between ethyl acetate and water
  4. washOrganic layer was washed with water and brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified on 50 g of silica gel column
  8. washeluting with 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-318f648bdb8443fd8e7553f459871710
出典データセット
uspto-grants-1995_07
特許番号
US05436233

関連ノート

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