Water → 2-Bromo-3-cyclohexyloxy pyridine

HRID 496809

反応式

HRID 496809 の反応式
[H-].[Na+].[Br:3][C:4]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][N:5]=1.Br[CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.O>CN(C)C=O>[Br:3][C:4]1[C:9]([O:10][CH:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)=[CH:8][CH:7]=[CH:6][N:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 7960Cyclohexyl bromideHCID 230702-Bromo-3-pyridinolHCID 24758Sodium hydride

生成物 1

HCID 223233602-Bromo-3-cyclohexyloxy pyridine収率 30%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Sodium hydride (160 mg) was dissolved in dimethylformamide (5 ml) and 2-bromo-3-pyridinol (500 mg) dissolved in dimethylformamide is slowly added dropwise. Then, bromocyclohexane (0.7 ml) was added to the solution and reacted for 5 hours at room temperature. Water was added to the suspension to dilute and extracted with ethyl acetate to separate an organic layer. The separated organic layer was dried with anhydrous magnesium sulfate and distilled under reduced pressure. As a result, 2-bromo-3-cyclohexyloxy pyridine (220 mg, yield: 30%) was obtained as an oil phase.

後処理

  1. additionis slowly added dropwise
  2. customreacted for 5 hours at room temperature
  3. additionto dilute
  4. extractionextracted with ethyl acetate
  5. customto separate an organic layer
  6. dry with materialThe separated organic layer was dried with anhydrous magnesium sulfate
  7. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-048d469ce30545f59c35fb3fe46cfc7d
出典データセット
uspto-grants-2005_09
特許番号
US06946558B2

関連ノート

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