吡啶 → 3-Bromo-5-(1-methanesulfonyl-pyrrolidin-2-yl)-pyridine

HRID 712753

反应方程式

HRID 712753 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.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:8]2[CH2:12][CH2:11][CH2:10][N:9]2[S:20]([CH3:19])(=[O:22])=[O:21])[CH:7]=1

参与物

5

反应物 3

HCID 1049吡啶HCID 31297甲基磺酰氯HCID 44038153-溴-5-(吡咯烷-2-基)吡啶

产物 1

HCID 1176674783-Bromo-5-(1-methanesulfonyl-pyrrolidin-2-yl)-pyridine收率 79%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

To a stirred solution of 3-bromo-5-(2-pyrrolidinyl)pyridine (0.2 g, 0.881 mmol) and pyridine (0.157 mL, 1.937 mmol) in DCM (1 mL) is added methanesulfonyl chloride in DCM (1 mL) dropwise. The mixture is stirred at room temperature for 2 h. The mixture is concentrated. The resulting crude product is purified by normal phase chromatography using 0-3% MeOH in DCM as the gradient to afford 3-bromo-5-(1-methanesulfonyl-pyrrolidin-2-yl)-pyridine (211.2 mg, 79% 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-b06947c158c34beab6694062b2731c89
来源数据集
uspto-grants-2015_11
专利号
US09181272B2

关联笔记

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