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Water → 6-(2,2-Difluoroethoxy)-5-methyl-3-nitro-2-pyridineamine

HRID 505389
ノート
印刷プレビュー

反応式

HRID 505389 の反応式
[F:1][CH:2]([F:5])[CH2:3][OH:4].[H-].[Na+].Cl[C:9]1[N:14]=[C:13]([NH2:15])[C:12]([N+:16]([O-:18])=[O:17])=[CH:11][C:10]=1[CH3:19].O>O1CCCC1>[F:1][CH:2]([F:5])[CH2:3][O:4][C:9]1[N:14]=[C:13]([NH2:15])[C:12]([N+:16]([O-:18])=[O:17])=[CH:11][C:10]=1[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 1361872,2-Difluoroethan-1-olHCID 218373796-Chloro-5-methyl-3-nitropyridin-2-amine

生成物 1

HCID 594298356-(2,2-Difluoroethoxy)-5-methyl-3-nitro-2-pyridineamine収率 96.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

2,2-Difluoro ethanol (418 mg, 5.1 mmol) was dissolved in tetrahydrofuran (15 ml), sodium hydride (60%) (180 mg, 4.5 mmol) was added thereto under nitrogen atmosphere, and the reaction mixture was stirred for 30 minutes at room temperature. A solution of 6-chloro-5-methyl-3-nitro-2-pyridineamine (600 mg, 3.20 mmol) in tetrahydrofuran (15 ml) was dropped, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution and extracted with ethyl acetate, and after washed with sodium bicarbonate solution, dried over magnesium sulfate. The residue obtained by evaporating the solvent was triturated with n-hexane to yield the title compound (685 mg, 3.1 mmol, 96%) as an orange solid.

後処理

  1. stirringthe mixture was stirred at room temperature overnight
  2. extractionextracted with ethyl acetate
  3. washafter washed with sodium bicarbonate solution
  4. dry with materialdried over magnesium sulfate
  5. customThe residue obtained
  6. customby evaporating the solvent
  7. customwas triturated with n-hexane

出典と根拠

ORDレコード
ord-19999b7d6a9a4f779d3e4170838ef18b
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781452B2

反応ノート

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