Potassium Carbonate → Methyl 2-methoxyimino-2-[3-chloro-2-(2-isopropoxy-6-trifluoromethylpyrimidin-4-yloxymethyl)phenyl]acetate

HRID 1584766ノート

反応式

HRID 1584766 の反応式
[CH:1]([O:4][C:5]1[N:10]=[C:9]([OH:11])[CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[N:6]=1)([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH3:22][O:23][N:24]=[C:25]([C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[CH2:37]Br)[C:26]([O:28][CH3:29])=[O:27]>CN(C)C=O>[CH3:22][O:23][N:24]=[C:25]([C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[CH2:37][O:11][C:9]1[CH:8]=[C:7]([C:12]([F:14])([F:15])[F:13])[N:6]=[C:5]([O:4][CH:1]([CH3:3])[CH3:2])[N:10]=1)[C:26]([O:28][CH3:29])=[O:27]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 73768265HCID 73768265、化合物HCID 178458952HCID 178458952、化合物

生成物 1

HCID 86754387Methyl 2-methoxyimino-2-[3-chloro-2-(2-isopropoxy-6-trifluoromethylpyrimidin-4-yloxymethyl)phenyl]acetate収率 61.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

3.3 g of 2-isopropoxy-4-hydroxy-6-trifluoromethylpyrimidine and 2.4 g of potassium carbonate are stirred at room temperature (about 25° C.) for 30 min in 100 ml of dimethyl formamide and the mixture is then treated dropwise in the course of 1 hour with a solution of 4.8 g of methyl 2-methoxyimino-2-[2-bromomethyl-3-chlorophenyl]acetate in 30 ml of dimethylformamide. After a further 8 hours at room temperature, the reaction mixture is added to ice water and the product is extracted using tert-butyl methyl ether. The combined ether phases are dried and concentrated. The crude product thus obtained is purified by chromatography (silica gel/toluene). 4.2 g of the title compound are obtained.

後処理

  1. extractionthe product is extracted
  2. dry with materialThe combined ether phases are dried
  3. concentrationconcentrated
  4. customThe crude product thus obtained
  5. customis purified by chromatography (silica gel/toluene)

出典と根拠

ORDレコード
ord-422a60950c844f1ca60bfa91707de3e6
出典データセット
uspto-grants-1999_08
特許番号
US05935965

反応ノート

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