2,4,6-Trichloropyrimidine → 2,6-dichloro-N-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidin-4-amine

HRID 1514330ノート

反応式

HRID 1514330 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[N:3]=1.[CH:10]1([C:13]2[NH:17][N:16]=[C:15]([NH2:18])[CH:14]=2)[CH2:12][CH2:11]1.C(N(C(C)C)CC)(C)C>C(O)CCC>[Cl:1][C:2]1[N:3]=[C:4]([NH:18][C:15]2[CH:14]=[C:13]([CH:10]3[CH2:12][CH2:11]3)[NH:17][N:16]=2)[CH:5]=[C:6]([Cl:8])[N:7]=1

参加物

5

反応物 3

HCID 773782,4,6-TrichloropyrimidineHCID 81531DiisopropylethylamineHCID 27580143-cyclopropyl-1H-pyrazol-5-amine

生成物 1

HCID 219910812,6-dichloro-N-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidin-4-amine収率 92.4%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2,4,6-trichloropyrimidine (30 g, 163 mmol), 5-cyclopropyl-1H-pyrazol-3-ylamine (20 g, 163 mmol), diisopropylethylamine (50 mL, 300 mmol) and 1-butanol (100 mL) was heated to 80° C. for 2 h. The solvents were removed on a rotary evaporator and the residue was taken up in ethyl acetate. The organic solution was washed with water and brine and dried over magnesium sulfate. The residue was concentrated on a rotary evaporator to give the desired product (40.7 g, 92%) as a light yellow solid.

後処理

  1. customThe solvents were removed on a rotary evaporator
  2. washThe organic solution was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe residue was concentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-cfbb234192134df697fe248679e9b00e
出典データセット
uspto-grants-2012_07
特許番号
US08222256B2

反応ノート

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