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Lithium hexamethyldisilazane → 2,6-Difluoro-N-{1-[(2-methyl-4-nitrophenyl)methyl]-1H-pyrazol-3-yl}benzamide

HRID 1946324
ノート
印刷プレビュー

反応式

HRID 1946324 の反応式
[F:1][C:2]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[C:3]=1[C:4]([NH:6][C:7]1[CH:11]=[CH:10][NH:9][N:8]=1)=[O:5].C[Si]([N-][Si](C)(C)C)(C)C.[Li+].Br[CH2:28][C:29]1[CH:34]=[CH:33][C:32]([N+:35]([O-:37])=[O:36])=[CH:31][C:30]=1[CH3:38]>C1COCC1>[F:1][C:2]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[C:3]=1[C:4]([NH:6][C:7]1[CH:11]=[CH:10][N:9]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([N+:35]([O-:37])=[O:36])=[CH:31][C:30]=2[CH3:38])[N:8]=1)=[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

5

反応物 3

HCID 2733832Lithium hexamethyldisilazaneHCID 126541471-(Bromomethyl)-2-methyl-4-nitrobenzeneHCID 178522346HCID 178522346、化合物

生成物 1

HCID 595478502,6-Difluoro-N-{1-[(2-methyl-4-nitrophenyl)methyl]-1H-pyrazol-3-yl}benzamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a solution of 2,6-difluoro-N-(1H-pyrazol-3-yl)benzamide (for a preparation see Intermediate 9)(1.5 g, 6.72 mmol) in THF (30 ml) at ambient temperature under nitrogen was added 1.0 M lithium bis(trimethylsilyl)amide in THF (6.5 ml, 6.50 mmol, Aldrich). The solution was stirred for 30 min. To the solution was added a solution of 1-(bromomethyl)-2-methyl-4-nitrobenzene (1.5 g, 6.52 mmol) in THF (20 ml). The resulting pale orange solution was stirred at ambient temperature under nitrogen over the weekend. The solvent was evaporated in vacuo and the residue partitioned between ethyl acetate (150 ml) and saturated aqueous sodium hydrogen carbonate (50 ml). The phases were separated and the aqueous layer washed with ethyl acetate (25 ml). The combined organic phases were dried (MgSO4), filtered and the solvent removed in vacuo to leave a yellow oil (2.87 g). The sample was loaded in dichloromethane and purified on silica 100 g using 0-100% ethyl acetate-cyclohexane. The appropriate fractions were combined and evaporated in vacuo to give the title compound as a white foam (1.6 g); LCMS: (System 4) MH+=373, tRET=2.65 min.

後処理

  1. customat ambient temperature
  2. stirringThe resulting pale orange solution was stirred at ambient temperature under nitrogen over the weekend
  3. customThe solvent was evaporated in vacuo
  4. customthe residue partitioned between ethyl acetate (150 ml) and saturated aqueous sodium hydrogen carbonate (50 ml)
  5. customThe phases were separated
  6. washthe aqueous layer washed with ethyl acetate (25 ml)
  7. dry with materialThe combined organic phases were dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-c022acd938ca4ac59de941a379368105
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399436B2

反応ノート

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