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

HRID 254216

반응식

HRID 254216 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0139c3b7b01d469282f5458362306b2c
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875606B2

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