吡啶 → 1-[2-(5-Bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone

HRID 712754

反应方程式

HRID 712754 反应方程式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:8]2[CH2:12][CH2:11][CH2:10][NH:9]2)[CH:7]=1.N1C=CC=CC=1.[C:19](OC(=O)C)(=[O:21])[CH3:20]>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[C:6]([CH:8]2[CH2:12][CH2:11][CH2:10][N:9]2[C:19](=[O:21])[CH3:20])[CH:5]=[N:4][CH:3]=1

参与物

5

反应物 3

HCID 1049吡啶HCID 7918乙酐HCID 44038153-溴-5-(吡咯烷-2-基)吡啶

产物 1

HCID 1176672401-[2-(5-Bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone收率 132%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

To a solution of 3-bromo-5-(2-pyrrolidinyl)pyridine (200 mg, 0.881 mmol) and pyridine (0.2 mL, 1.96 mmol) in DCM (1 mL) in a 8-mL vial is added acetic anhydride (0.093 mL, 0.969 mmol) dropwise. The mixture is stirred at room temperature for 2.5 h. The mixture is concentrated. The resulting crude product is purified by normal phase chromatography using 0-4.5% MeOH in DCM as the gradient to afford 1-[2-(5-bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone (313 mg, 83% yield).

后处理

  1. concentrationThe mixture is concentrated
  2. customThe resulting crude product is purified by normal phase chromatography

来源与证据

ORD记录
ord-621fe542518d4dd4a7d446037a497fb3
来源数据集
uspto-grants-2015_11
专利号
US09181272B2

关联笔记

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