p-Fluoronitrobenzene → methyl-[9-(4-nitrophenyl)-9H-purin-6-yl]amine

HRID 1912854노트

반응식

HRID 1912854 반응식
[CH3:1][NH:2][C:3]1[N:11]=[CH:10][N:9]=[C:8]2[C:4]=1[N:5]=[CH:6][NH:7]2.[H-].[Na+].F[C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1>CS(C)=O.CCCCCC.O>[CH3:1][NH:2][C:3]1[N:11]=[CH:10][N:9]=[C:8]2[C:4]=1[N:5]=[CH:6][N:7]2[C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1

참가 물질

7

반응물 3

HCID 9590p-FluoronitrobenzeneHCID 24758Sodium hydrideHCID 178482413HCID 178482413, 화합물

생성물 1

HCID 23155308methyl-[9-(4-nitrophenyl)-9H-purin-6-yl]amine수율 83%

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 8058Hexane용매

실험 절차

In 120 mL of dimethyl sulfoxide, 10.78 g (80 mmol) of methyl-(9H-purin-6-yl)amine was dissolved, and 1.98 g (82.5 mmol) of sodium hydride (60%) after washing with hexane was added thereto and the mixture solution was stirred at room temperature for one hour. To the reaction solution, 13.0 g (92 mmol) of 4-fluoronitrobenzene was added dropwise and the resulting solution was stirred at 80° C. for two hours. The reaction solution was diluted with 300 mL of water, and the crystal deposited was collected on a filter, then washed with 100 mL of water and subsequently with 500 mL of ethanol, and vacuum dried to obtain 16.14 g (83%) of a target product as a yellow solid.

후처리

  1. additionwas added
  2. stirringthe resulting solution was stirred at 80° C. for two hours
  3. customthe crystal deposited was collected on a filter
  4. washwashed with 100 mL of water and subsequently with 500 mL of ethanol, and vacuum
  5. customdried

출처 및 근거

ORD 기록
ord-5751a6afb639405984d55a321dff887b
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609656B2

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