반응 #1119361

반응 방정식

3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbonyl chloride

potassium carbonate

N-methylallylamine

→

N-Methyl-N-(2-propenyl)-3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide hydrate

용매

tetrahydrofuran

water

반응 조건

후처리

1. 1
   workup.ADDITIONa piece of ice was added
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITcontinued for 15 hr
4. 4
   기타the oil which separated
5. 5
   추출was extracted into methylene chloride (2×50 ml)
6. 6
   건조The combined extracts were dried over magnesium sulfate
7. 7
   농축concentrated in vacuo (3.7 g)
8. 8
   기타The crude oil was chromatographed on a 75 g silica gel column
9. 9
   세척by eluting with chloroform
10. 10
    세척After the first crude material was washed from the column the three product fractions
11. 11
    농축concentrated in vacuo
12. 12
    기타to yield 3 g (97%) of water-like oil

실험 절차

A stirred mixture of 2.8 g (0.01 mole) of 3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbonyl chloride and 1.4 g (0.01 mole) of potassium carbonate in 20 ml of tetrahydrofuran was treated with 0.72 g (0.01 mole) of N-methylallylamine. After stirring for 15 minutes, a piece of ice was added and stirring continued for 15 hr. The reaction mixture was diluted with water and the oil which separated was extracted into methylene chloride (2×50 ml). The combined extracts were dried over magnesium sulfate and concentrated in vacuo (3.7 g). The crude oil was chromatographed on a 75 g silica gel column by eluting with chloroform. After the first crude material was washed from the column the three product fractions were combined and concentrated in vacuo, to yield 3 g (97%) of water-like oil.

출처