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

HRID 507671ノート

反応式

HRID 507671 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d2286de9ef54af1b45747777142b17a
出典データセット
uspto-grants-2010_08
特許番号
US07786132B2

反応ノート

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