Dimethylformamide → (1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-yl)-methanethiol

HRID 254216

反応式

HRID 254216 の反応式
Br[CH2:2][C:3]1[C:4]([C:13]([F:16])([F:15])[F:14])=[N:5][N:6]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:7]=1[Cl:8].CN(C)C=O.O.[SH-:23].[Na+]>C(OCC)C>[C:9]([N:6]1[C:7]([Cl:8])=[C:3]([CH2:2][SH:23])[C:4]([C:13]([F:16])([F:15])[F:14])=[N:5]1)([CH3:12])([CH3:11])[CH3:10]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 16211346Sodium hydrosulfide hydrateHCID 178628684-bromomethyl-1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazole

生成物 1

HCID 17862846(1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-yl)-methanethiol収率 87%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

43.5 g (136.1 mmoles) of 4-bromomethyl-1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazole was added to 300 ml of a N,N-dimethylformamide solution containing 21.8 g (272.2 mmoles) of sodium hydrosulfide hydrate (purity: 70%). The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water and extraction with diethyl ether was conducted. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein, to obtain 32.3 g (yield: 87.0%) of (1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-yl)-metha-nethiol.

後処理

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to reduced pressure distillation
  7. customto remove the solvent

出典と根拠

ORDレコード
ord-0139c3b7b01d469282f5458362306b2c
出典データセット
uspto-grants-2011_01
特許番号
US07875606B2

関連ノート

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