Potassium Carbonate → HCID 68768624, 화합물

HRID 1172087노트

반응식

HRID 1172087 반응식
O.[SH-].[Na+].[CH3:4][C:5]1([CH3:15])[O:9][N:8]=[C:7]([S:10]([CH2:13][CH3:14])(=O)=O)[CH2:6]1.C(=O)([O-])[O-].[K+].[K+].C(S([O-])=O)O.[Na+].BrCC1[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.O>[Cl:35][C:34]1[N:33]([CH3:36])[N:32]=[C:31]([C:37]([F:40])([F:39])[F:38])[C:14]=1[CH2:13][S:10][C:7]1[CH2:6][C:5]([CH3:15])([CH3:4])[O:9][N:8]=1

참가 물질

8

반응물 5

HCID 11430Potassium CarbonateHCID 114259074-bromomethyl-5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazoleHCID 16211346Sodium hydrosulfide hydrateHCID 178629235,5-Dimethyl-3-ethylsulfonyl-2-isoxazolineHCID 23689980Sodium Formaldehyde Sulfoxylate

생성물 1

HCID 68768624HCID 68768624, 화합물수율 80.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

5.59 g of sodium hydrosulfide hydrate (purity: 70%, 69.8 mmoles) was added, at room temperature, to a solution of 6.84 g (35.8 mmoles) of 5,5-dimethyl-3-ethanesulfonyl-2-isoxazoline dissolved in 200 ml of N,N-dimethylformamide. The mixture was stirred for 1 hour. To the reaction mixture, were added 4.94 g (35.8 mmoles) of anhydrous potassium carbonate, 5.51 g (35.8 mmoles) of Rongalit and further 9.46 g (34.1 mmoles) of 4-bromomethyl-5-chloro-1-methyl-3-trifluoromethyl-1H-pyrazole. The resulting mixture was stirred at room temperature over one night to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 8.97 g (yield: 80.3%) of 3-(5-chloro-1-methyl-3-trifluoromethylpyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazoline.

후처리

  1. stirringThe resulting mixture was stirred at room temperature over one night
  2. customto give rise
  3. customto a reaction
  4. customAfter confirmation of the completion of the reaction
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe resulting organic layer was washed with water
  7. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  8. distillationThe resulting solution was subjected to vacuum distillation
  9. customto remove the solvent
  10. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-0bb259f9c18946b2a9ee3cecb74c7131
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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