碳酸钾 → 3-chloro-N-methylpropane-1-sulfonamide

HRID 36876

反应方程式

HRID 36876 反应方程式
[Cl:1][CH2:2][CH2:3][CH2:4][S:5](Cl)(=[O:7])=[O:6].Cl.[CH3:10][NH2:11].C(=O)([O-])[O-].[K+].[K+]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(OCC)(=O)C>[CH3:10][NH:11][S:5]([CH2:4][CH2:3][CH2:2][Cl:1])(=[O:7])=[O:6]

参与物

6

反应物 3

HCID 11430碳酸钾HCID 154103-氯丙烷磺酰氯HCID 6364545甲胺盐酸盐

产物 1

HCID 102412533-chloro-N-methylpropane-1-sulfonamide收率 74%

试剂、催化剂与溶剂 2

HCID 5963苄基三甲基氯化铵催化剂HCID 8857乙酸乙酯溶剂

实验过程

3-Chloropropylsulfonyl chloride 1 (6.8 g,94.9 mmol), methylamine hydrochloride (13.5 g,200 mmol), and potassium carbonate (27.6 g,200 mmol) were added in turn to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg), the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.

后处理

  1. dry with materialdried over anhydrous sodium sulfate
  2. filtrationThe mixture was filtered through a small amount of silica gel
  3. concentrationthe filtrate was concentrated in vacuo

来源与证据

ORD记录
ord-88506e12a7c6447fb7f6d563c2d9e044
来源数据集
uspto-grants-1995_05
专利号
US05418230

关联笔记

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