Triethylamine → 6-Trifluoromethoxy-1-trifluoromethylsulphenylindazole

HRID 868175ノート

反応式

HRID 868175 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 137130126-Trifluoromethoxy-1-trifluoromethylsulphenylindazole

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ffd70e6dcf6542288e1094786099fbe2
出典データセット
uspto-grants-1988_10
特許番号
US04778511

反応ノート

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