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Sodium Methoxide → HCID 178527384、化合物

HRID 990621
ノート
印刷プレビュー

反応式

HRID 990621 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 12056494HCID 12056494、化合物

生成物 1

HCID 178527384HCID 178527384、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2a3c01b2d8084e45bfdc3dfe07098ee6
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06461997B1

反応ノート

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