Water → 1-Methyl-5-difluoromethoxy-4-chloro-3-(2-fluoro-4-chlorophenyl)pyrazole

HRID 634561노트

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HRID 634561 반응식
[CH3:1][N:2]1[C:6]([O:7][CH:8]([F:10])[F:9])=[CH:5][C:4]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[F:18])=[N:3]1.[Cl:19]N1C(=O)CCC1=O.O>CN(C)C=O>[CH3:1][N:2]1[C:6]([O:7][CH:8]([F:9])[F:10])=[C:5]([Cl:19])[C:4]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[F:18])=[N:3]1

참가 물질

5

반응물 3

HCID 962WaterHCID 31398ChlorosuccinimideHCID 11357876HCID 11357876, 화합물

생성물 1

HCID 114383281-Methyl-5-difluoromethoxy-4-chloro-3-(2-fluoro-4-chlorophenyl)pyrazole수율 98.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 16.2 grams (0.059 mole) of 1-methyl-5-difluoromethoxy-3-(2-fluoro-4-chlorophenyl)pyrazole and 8.5 grams (0.064 mole) of N-chlorosuc-cinimide in about 500 mL of N,N-dimethylformamide was stirred at ambient temperature for about 18 hours. After this time the reaction mixture was poured into about 1600 mL of water and then extracted with two portions of diethyl ether. The combined extracts were washed with one portion of aqueous 10% lithium chloride and two portions of a saturated aqueous solution of sodium chloride. The organic layer was dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 18.0 grams of 1-methyl-5-difluoromethoxy-4-chloro-3-(2-fluoro-4-chlorophenyl)pyrazole. The NMR spectrum was consistent with the proposed structure.

후처리

  1. extractionextracted with two portions of diethyl ether
  2. washThe combined extracts were washed with one portion of aqueous 10% lithium chloride and two portions of a saturated aqueous solution of sodium chloride
  3. dry with materialThe organic layer was dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0d9fe556128a4b0b8708ed7d0d406e3c
출처 데이터셋
uspto-grants-2001_02
특허 번호
USH0001942H1

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