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

HRID 2171262ノート

反応式

HRID 2171262 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b3b8573fc6f8424fb51a58e7edfbc329
出典データセット
uspto-grants-2015_06
特許番号
US09051310B2

反応ノート

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