反応 #2122513

反応方程式

Compound 2

2-methylbenzothiazole-6-sulfonyl chloride

piperidine

hexane

→

Compound 3

収率 74.2%

N-(2-methylbenzothiazole-6-sulfonyl)piperidine

収率 74.2%

溶媒

ethyl acetate

chloroform

chloroform

反応条件

後処理

1. 1
   洗浄The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml)
2. 2
   乾燥The organic layer was dried with sodium sulfate
3. 3
   その他evaporated
4. 4
   その他The sticky white solid thus obtained
5. 5
   その他The white solid that precipitated
6. 6
   その他was collected
7. 7
   洗浄washed with hexane
8. 8
   その他dried

実験手順

A solution of Compound 2 (2.5 g, 10 mmol) in chloroform (15 ml) was added drop wise to a solution of piperidine (1.7 g, 20.0 mmol) in chloroform (10 ml). The combined mixture was stirred at room temperature for 1 hour. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was dried with sodium sulfate and evaporated. The sticky white solid thus obtained was dissolved in ca. 5 ml of hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was collected, washed with hexane and dried to yield 2.2 g (74%) of Compound 3, Rf=0.28 (30% ethyl acetate in hexane). The structure of Compound 3 is given below:

出典