Ethyl Acetate → 3-(Cyclopropyl(2,6-dichloropyrimidin-4-yl)amino)propan-1-ol

HRID 930801노트

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HRID 930801 반응식
[CH:1]1([NH:4][CH2:5][CH2:6][CH2:7][OH:8])[CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.[Cl:18][C:19]1[N:24]=[C:23](Cl)[CH:22]=[C:21]([Cl:26])[N:20]=1.CCOC(C)=O>CN(C)C=O>[CH:1]1([N:4]([C:23]2[CH:22]=[C:21]([Cl:26])[N:20]=[C:19]([Cl:18])[N:24]=2)[CH2:5][CH2:6][CH2:7][OH:8])[CH2:3][CH2:2]1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 773782,4,6-TrichloropyrimidineHCID 81531DiisopropylethylamineHCID 545472183-(Cyclopropylamino)propan-1-ol

생성물 1

HCID 903031303-(Cyclopropyl(2,6-dichloropyrimidin-4-yl)amino)propan-1-ol수율 23.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

To a solution of 3-(cyclopropylamino)propan-1-ol (7 g, 60.8 mmol) and Hunig's base (31.8 mL, 182 mmol) in N,N-dimethylformamide (20 mL), was added 2,4,6-trichloropyrimidine (7.10 mL, 60.8 mmol), stirred for 3 h at 0° C. Then, EtOAc (150 mL) was added, and the organic phase was washed with water, brine, dried over Na2SO4, and concentrated. Purification via FC afforded the title compound (3.8 g).

후처리

  1. washthe organic phase was washed with water, brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customPurification via FC

출처 및 근거

ORD 기록
ord-06fbd6224ace4d6caecebf135a66ebc8
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296755B2

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