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2,4-Dichloro-5-(trifluoromethyl)pyrimidine → 4-Chloro-2-[6-(dimethylphosphoryl)-2-methoxypyridin-3-yl]-5-(trifluoromethyl)pyrimidine

HRID 1471996
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HRID 1471996 반응식
[CH3:1][P:2]([C:5]1[N:10]=[C:9]([O:11][CH3:12])[C:8](N)=[CH:7][CH:6]=1)([CH3:4])=[O:3].Cl[C:15]1[N:20]=[C:19]([Cl:21])[C:18]([C:22]([F:25])([F:24])[F:23])=[CH:17][N:16]=1>CN(C)C(=O)C.C(N(C(C)C)CC)(C)C>[Cl:21][C:19]1[C:18]([C:22]([F:24])([F:23])[F:25])=[CH:17][N:16]=[C:15]([C:8]2[C:9]([O:11][CH3:12])=[N:10][C:5]([P:2]([CH3:4])([CH3:1])=[O:3])=[CH:6][CH:7]=2)[N:20]=1
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참가 물질

5

반응물 2

HCID 27827742,4-Dichloro-5-(trifluoromethyl)pyrimidineHCID 67052694(5-Amino-6-methoxypyridin-2-yl)dimethylphosphine oxide

생성물 1

HCID 866687954-Chloro-2-[6-(dimethylphosphoryl)-2-methoxypyridin-3-yl]-5-(trifluoromethyl)pyrimidine

시약·촉매·용매 2

HCID 31374Dimethylacetamide용매HCID 81531Diisopropylethylamine용매

실험 절차

A suspension of 6-(dimethylphosphoryl)-2-methoxypyridin-3-ylamine (prepared in Example 32: 2.2 mmol) in 15 mL of N,N-Dimethylacetamide and 3.6 mL of Diisopropylethylamine, is allowed to stirred at room temperature for 15 minutes until a clear solution is obtained. 2,4-Dichloro-5-(trifluoromethyl)pyrimidine (5.7 g, 2.6 mmol) is added in four portions over 5 minutes. The reaction mixture is stirred at 60 degrees for 1 hour. The reaction mixture is cooled to room temperature and filtered to obtain a white solid. The white solid is washed with 50 mL of water three times and followed by 50 mL of Ethyl ether three times. The white solid is dried under vacuum to yield 4-chloro-2-[6-(dimethylphosphoryl)-2-methoxypyridin-3-yl]-5-(trifluoromethyl)pyrimidine.

후처리

  1. customis obtained
  2. stirringThe reaction mixture is stirred at 60 degrees for 1 hour
  3. temperatureThe reaction mixture is cooled to room temperature
  4. filtrationfiltered
  5. customto obtain a white solid
  6. washThe white solid is washed with 50 mL of water three times
  7. customThe white solid is dried under vacuum

출처 및 근거

ORD 기록
ord-148fe0917bc849e0ba6a74dd04d62fce
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012462B2

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