Triethylamine → 6-Trifluoromethoxy-1-trifluoromethylsulphenylindazole

HRID 868175노트

반응식

HRID 868175 반응식
[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][NH:10]2)=[CH:6][CH:5]=1.C(N(CC)CC)C.[F:22][C:23]([F:27])([F:26])[S:24]Cl>C1(C)C=CC=CC=1>[F:14][C:2]([F:1])([F:13])[O:3][C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][N:10]2[S:24][C:23]([F:27])([F:26])[F:22])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 67900Methanesulfenyl chloride, trifluoro-HCID 137129976-(Trifluoromethoxy)-1H-indazole

생성물 1

HCID 137130126-Trifluoromethoxy-1-trifluoromethylsulphenylindazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

20.2 g (0.1 mole) of 6-trifluoromethoxyindazole and 10.1 g (0.1 mole) of triethylamine in 125 ml of toluene are heated to 80° to 85° C., and 13.6 g (0.1 mole) of trifluoromethanesulphenyl chloride are then passed in the course of one hour and the mixture is stirred for a further hour at this temperature. After cooling, the precipitated triethylamine hydrochloride is filtered off with suction and rinsed with toluene. The filtrate, combined with the wash liquor, is washed twice with water. After drying (MgSO4) the volatile constituents are removed by distillation under a water pump vacuum. The oily crude product is purified by distillation under an oil pump vacuum. Boiling point 62°/0.05 mbar. Yield: 16.2 g (46% of theory).

후처리

  1. customare then passed in the course of one hour
  2. temperatureAfter cooling
  3. filtrationthe precipitated triethylamine hydrochloride is filtered off with suction
  4. washrinsed with toluene
  5. washis washed twice with water
  6. dry with materialAfter drying (MgSO4) the volatile constituents
  7. customare removed by distillation under a water pump vacuum
  8. distillationThe oily crude product is purified by distillation under an oil pump vacuum

출처 및 근거

ORD 기록
ord-ffd70e6dcf6542288e1094786099fbe2
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778511

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