Water → 2-Chloro-4-hydrazinylpyrimidine

HRID 601004노트

반응식

HRID 601004 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 160921982-Chloro-4-hydrazinylpyrimidine수율 23%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f97b039f0edf4fbd92c86121064356ce
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902239B2

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