Potassium Carbonate → HCID 11314445、化合物

HRID 254203

反応式

HRID 254203 の反応式
O.[SH-].[Na+].[Cl:4][CH2:5][C:6]1([CH3:15])[O:10][N:9]=[C:8]([S:11]([CH3:14])(=O)=O)[CH2:7]1.C(=O)([O-])[O-].[K+].[K+].C(S([O-])=O)O.[Na+].BrC[C:30]1[C:31]([C:37]([F:40])([F:39])[F:38])=[N:32][N:33]([CH3:36])[C:34]=1[Cl:35]>CN(C)C=O.C(OCC)(=O)C.O>[Cl:35][C:34]1[N:33]([CH3:36])[N:32]=[C:31]([C:37]([F:40])([F:39])[F:38])[C:30]=1[CH2:14][S:11][C:8]1[CH2:7][C:6]([CH2:5][Cl:4])([CH3:15])[O:10][N:9]=1

参加物

9

反応物 5

HCID 11430Potassium CarbonateHCID 111952063-Methylsulfonyl-5-chloromethyl-5-methyl-2-isoxazolineHCID 114259074-bromomethyl-5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazoleHCID 16211346Sodium hydrosulfide hydrateHCID 23689980Sodium Formaldehyde Sulfoxylate

生成物 1

HCID 11314445HCID 11314445、化合物収率 100%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1.2 g (15.0 mmoles) of sodium hydrosulfide hydrate (purity: 70%) was added into a solution of 2.1 g (10.0 mmoles) of 5-chloromethyl-5-methyl-3-methylsulfonyl-2-isoxazoline dissolved in 20 ml of N,N-dimethylformamide. The mixture was stirred for 2 hours. Then, there were added 2.1 g (15.0 mmoles) of anhydrous potassium carbonate, 2.3 g (15.0 mmoles) of Rongalit and 2.8 g (10.0 mmoles) of 4-bromomethyl-5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazole. The mixture was stirred at room temperature for 2 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water and extraction with ethyl acetate was conducted. The resulting organic layer was washed with an aqueous sodium chloride solution, followed by drying over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 3.3 g (yield: 100.0%) of 3-(5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5-chloromethyl-5-methyl-2-isoxazoline.

後処理

  1. stirringThe mixture was stirred at room temperature for 2 hours
  2. customto give rise
  3. customto a reaction
  4. customAfter the completion of the reaction
  5. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  6. dry with materialby drying over anhydrous magnesium sulfate
  7. distillationThe resulting solution was subjected to reduced pressure distillation
  8. customto remove the solvent
  9. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f5449b15f7f64e24b9378363a2e8677e
出典データセット
uspto-grants-2011_01
特許番号
US07875606B2

関連ノート

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