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

HRID 634561ノート

反応式

HRID 634561 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 31398ChlorosuccinimideHCID 11357876HCID 11357876、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0d9fe556128a4b0b8708ed7d0d406e3c
出典データセット
uspto-grants-2001_02
特許番号
USH0001942H1

反応ノート

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