Triethylamine → N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide

HRID 238671ノート

反応式

HRID 238671 の反応式
[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][NH:5][N:4]=1.C(N(CC)CC)C.[CH3:17][N:18]([CH3:23])[S:19](Cl)(=[O:21])=[O:20]>ClCCl.C(OCC)C>[CH3:17][N:18]([CH3:23])[S:19]([N:5]1[CH:6]=[CH:7][C:3]([C:2]([F:9])([F:8])[F:1])=[N:4]1)(=[O:21])=[O:20]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 83372Dimethylsulphamoyl chlorideHCID 18070343-(Trifluoromethyl)pyrazole

生成物 1

HCID 66826467N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide収率 99.5%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-trifluoromethylpyrazole (5.0 g, 36 mmol), triethylamine (7.0 mL, 50 mmol) in dichloromethane (40 mL) was added dimethylsulfamoyl chloride (5.5 mL, 51 mmol), and the reaction mixture was heated at reflux for 2 days. The resulting mixture was cooled to ambient temperature and filtered through a pad of silica gel using dichloromethane as eluent. The filtrate was then concentrated under reduced pressure to give an amber residue. The resulting residue was dissolved in diethyl ether. The ether solution was washed with water, dried (MgSO4), and concentrated under reduced pressure to give 8.71 g of the title compound.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 2 days
  3. filtrationfiltered through a pad of silica gel
  4. concentrationThe filtrate was then concentrated under reduced pressure
  5. customto give an amber residue
  6. washThe ether solution was washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b76b1bad2d0d4129aedbe7933402080a
出典データセット
uspto-grants-2014_02
特許番号
US08642634B2

反応ノート

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