Pyrazole → 5-Bromo-2-(1H-pyrazol-1-yl)pyrimidine

HRID 2171262노트

반응식

HRID 2171262 반응식
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.C(=O)([O-])[O-].[Cs+].[Cs+].CC(N(C)C)=O.[Br:18][C:19]1[CH:20]=[N:21][C:22](Cl)=[N:23][CH:24]=1>O>[Br:18][C:19]1[CH:20]=[N:21][C:22]([N:1]2[CH:5]=[CH:4][CH:3]=[N:2]2)=[N:23][CH:24]=1

참가 물질

6

반응물 4

HCID 1048PyrazoleHCID 10796Cesium carbonateHCID 31374DimethylacetamideHCID 6066655-Bromo-2-chloropyrimidine

생성물 1

HCID 457897835-Bromo-2-(1H-pyrazol-1-yl)pyrimidine수율 126.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

Pyrazole (130 mg) and cesium carbonate (610 mg) were added to a DMAc (10 ml) solution containing 5-bromo-2-chloropyrimidine (300 mg), followed by stirring at 120° C. for 0.5 hours. The reaction mixture was adjusted to room temperature and water was added to the mixture. Next, the organic layers were collected, washed with saturated saline, and dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure and a yellow solid of 5-bromo-2-(pyrazol-1-yl)pyrimidine (440 mg) was thus obtained.

후처리

  1. customwas adjusted to room temperature
  2. customNext, the organic layers were collected
  3. washwashed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled away under reduced pressure

출처 및 근거

ORD 기록
ord-b3b8573fc6f8424fb51a58e7edfbc329
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051310B2

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