Dimethylformamide → HCID 86746158、化合物

HRID 1886326

反応式

HRID 1886326 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)[CH:7]=[CH:6][C:5]=1[OH:21].Cl[C:23]1[CH:28]=[CH:27][C:26](CCl)=[CH:25][N:24]=1.[CH3:31]N(C)C=O>>[Cl:3][C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:19])([F:20])[F:18])[CH:12]=2)[CH:7]=[CH:6][C:5]=1[O:21][CH2:31][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=1

参加物

5

反応物 4

HCID 6228Dimethylformamide3 回HCID 24758Sodium hydrideHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 189667272-Chloro-4-(3-trifluoromethylphenoxy)phenol

生成物 1

HCID 86746158HCID 86746158、化合物

実験手順

To a solution 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there was added dropwise a solution of 0.50 g of 2-chloro-4-(3-trifluoromethylphenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.28 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide was added thereto at room temperature, followed by stirring at the same temperature for 10 hours. The reaction mixture was poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 2-chloro-5[[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine.

後処理

  1. temperatureice-cooling
  2. customat room temperature
  3. stirringby stirring at the same temperature for 10 hours
  4. extractionextracted twice with 100 ml of ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7408419a1219444fa4bd65ef2386ffca
出典データセット
uspto-grants-1992_09
特許番号
US05151428

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