Water → 2-Chloro-4-hydrazinylpyrimidine

HRID 601004ノート

反応式

HRID 601004 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.C(N(CC)CC)C.[NH2:16][NH2:17].O>C(O)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:16][NH2:17])[CH:5]=[CH:4][N:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 9321HydrazineHCID 775312,4-Dichloropyrimidine

生成物 1

HCID 160921982-Chloro-4-hydrazinylpyrimidine収率 23%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2,4-dichloropyrimidine (1.49 g, 10.0 mmol) in ethanol (25 mL) was added triethylamine (2.02 g, 2.78 mL, 20.0 mmol) and hydrazine (321 mg, 0.321 mL, 10.0 mmol). The mixture was stirred at room temperature for 2 h. Water was added and the mixture was extracted with dichloromethane. The organic layer was dried over MgSO4, concentrated. The residue was purified by silica gel column chromatograghy eluted with methanol:dichloromethane (2 to 5% methanol) to give (2-chloro-pyrimidin-4-yl)-hydrazine (330 mg, 23%) as a white solid. MS (ES+): m/z=144.9.

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. dry with materialThe organic layer was dried over MgSO4
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatograghy
  5. washeluted with methanol

出典と根拠

ORDレコード
ord-f97b039f0edf4fbd92c86121064356ce
出典データセット
uspto-grants-2011_03
特許番号
US07902239B2

反応ノート

読み込み中…