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

HRID 1471996
ノート
印刷プレビュー

反応式

HRID 1471996 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 31374Dimethylacetamide溶媒HCID 81531Diisopropylethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-148fe0917bc849e0ba6a74dd04d62fce
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012462B2

反応ノート

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