Potassium Carbonate → 1-(2-(5-Bromo-4-(5-chlorothiophen-2-yl)pyrimidin-2-ylamino)ethyl)imidazolidin-2-one

HRID 507671

반응식

HRID 507671 반응식
[Br:1][C:2]1[C:3]([C:9]2[S:10][C:11]([Cl:14])=[CH:12][CH:13]=2)=[N:4][C:5](Cl)=[N:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[NH2:21][CH2:22][CH2:23][N:24]1[CH2:28][CH2:27][NH:26][C:25]1=[O:29].C(=O)(O)[O-].[Na+]>CN1CCCC1=O>[Br:1][C:2]1[C:3]([C:9]2[S:10][C:11]([Cl:14])=[CH:12][CH:13]=2)=[N:4][C:5]([NH:21][CH2:22][CH2:23][N:24]2[CH2:28][CH2:27][NH:26][C:25]2=[O:29])=[N:6][CH:7]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 80480N-(2-Aminoethyl)ethyleneureaHCID 516892Sodium BicarbonateHCID 574288335-Bromo-2-chloro-4-(5-chlorothiophen-2-yl)pyrimidine

생성물 1

HCID 602046201-(2-(5-Bromo-4-(5-chlorothiophen-2-yl)pyrimidin-2-ylamino)ethyl)imidazolidin-2-one

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

5-Bromo-2-chloro-4-(5-chlorothiophen-2-yl)pyrimidine (0.4g, 1.3 mmol), N-methyl pyrrolidone (3 mL), potassium carbonate (0.358 g, 2.6 mmol) and 1-(2-aminoethyl)-imidazolidin-2-one (0.2 g, 1.54 mmol) were all placed in a microwave tube. The reaction was heated to 150° C. for 20 min in a Personal Chemistry microwave. A saturated solution of sodium bicarbonate was added to the reaction mixtue, which was extracted three times with dichloromethane. The organic layer was dried with sodium sulfate and purified by flash chromatography on silica gel using gradient of 0 to 10% methanol in dichloromethane to obtain a white solid. Yield=0.41 g. MS (M+H)+ 402/404.

후처리

  1. customall placed in a microwave tube
  2. extractionwas extracted three times with dichloromethane
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. custompurified by flash chromatography on silica gel using gradient of 0 to 10% methanol in dichloromethane
  5. customto obtain a white solid

출처 및 근거

ORD 기록
ord-9d2286de9ef54af1b45747777142b17a
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786132B2

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