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

HRID 1510406노트

반응식

HRID 1510406 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8139f89afe3845aeb650b0654ced279c
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211929B2

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