Chlorosuccinimide → 1-Phenyl-3-trifluoromethyl-4-chloropyrazole

HRID 1289842

반응식

HRID 1289842 반응식
[C:1]1([N:7]2[C:11](O)=[CH:10][C:9]([C:13]([F:16])([F:15])[F:14])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:17]N1C(=O)CCC1=O>C(O)(C(F)(F)F)=O.C(O)(=O)C.C(O)(=O)C>[C:1]1([N:7]2[CH:11]=[C:10]([Cl:17])[C:9]([C:13]([F:16])([F:15])[F:14])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 178516151HCID 178516151, 화합물

생성물 1

HCID 189225581-Phenyl-3-trifluoromethyl-4-chloropyrazole수율 22.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 23437676Trifluoroacetic acid acetate용매

실험 절차

A mixture of 2.28 g (10 mmol) of 1-phenyl-3-trifluoromethyl-5-hydroxypyrazole and 1.6 g (12 mmol) of N-chlorosuccinimide in 8 ml of 20% TFA/acetic acid and 32 mL of acetic acid was stirred at room temperature for 16 hours and diluted with ice/water with cooling. The white precipitate was filtered and purified by column chromatography (silica gel; 20-33% ethyl acetate/hexane) to afford 550 mg (21%) of 1-phenyl-3-trifluoromethyl-4-chloropyrazole as a solid.

후처리

  1. temperaturewith cooling
  2. filtrationThe white precipitate was filtered
  3. custompurified by column chromatography (silica gel; 20-33% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-eabfc51b685b49549795800784b0c78b
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750550

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