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Sodium Methoxide → HCID 178527384, 화합물

HRID 990621
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HRID 990621 반응식
[Br:1][C:2]([F:19])([F:18])[S:3]([C:6]1[N:10]=[CH:9][N:8](C(=O)N(CC)CC)[N:7]=1)(=[O:5])=[O:4].C[O-].[Na+]>CO>[Br:1][C:2]([F:18])([F:19])[S:3]([C:6]1[N:10]=[CH:9][NH:8][N:7]=1)(=[O:4])=[O:5]
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참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 12056494HCID 12056494, 화합물

생성물 1

HCID 178527384HCID 178527384, 화합물수율 61.9%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of 7 g (0.019 mol) 3-(bromodifluoromethylsulfonyl)-1-(N,N-diethylcarbamoyl)-1,2,4-triazole, prepared as in Example 1, in 50 ml methanol at room temperature was added 6.7 ml (0.029 mol) of a 25% w/v solution of sodium methoxide in methanol and the mixture was stirred for 2 h. The reaction mixture was then evaporated and the residue was triturated with ether. The resulting solid was collected by filtration, washed with ether and air-dried. A solution of the above solid in 50 ml water was acidified with concentrated hydrochloric acid and the mixture was extracted with ethyl acetate. The resulting organic layer was washed with saturated sodium chloride solution, dried over MgSO4 and evaporated to give 3.08 g (61% yield) of the desired 3-(bromodifluoromethylsulfonyl)-1,2,4-triazole as a white solid with a melting point of 176-177° C.

후처리

  1. customThe reaction mixture was then evaporated
  2. customthe residue was triturated with ether
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with ether
  5. customair-dried
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe resulting organic layer was washed with saturated sodium chloride solution
  8. dry with materialdried over MgSO4
  9. customevaporated

출처 및 근거

ORD 기록
ord-2a3c01b2d8084e45bfdc3dfe07098ee6
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06461997B1

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