반응 #8942

반응 방정식

4-benzylpiperazine

NEt3

ethyl acetate hexane

benzyl 3-chlorosulfonyl-2(R)-methylpropionate

→

pure product

benzyl 3-(4-benzylpiperizin-1-yl sulfonyl)-2(R)-methylpropionate

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet
2. 2
   농축then concentrated in vacuo
3. 3
   기타partitioned between ethyl acetate and saturated sodium bicarbonate
4. 4
   세척The combined organics were washed with brine
5. 5
   건조dried over Na2SO4
6. 6
   농축concentrated in vacuo
7. 7
   기타to yield 3.4 g crude product

실험 절차

A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet was charged with 2.5 g benzyl 3-chlorosulfonyl-2(R)-methylpropionate in 25 mL CH2Cl2. The solution was cooled to 0° C. and charged with 1.57 mL (1.0 eq.) 4-benzylpiperazine and 1.26 mL NEt3. The reaction was stirred for 1 hour then concentrated in vacuo and partitioned between ethyl acetate and saturated sodium bicarbonate. The combined organics were washed with brine, dried over Na2SO4, and concentrated in vacuo to yield 3.4 g crude product. Flash chromatography (80:20 ethyl acetate/hexane) yielded 3.0 g pure product.

출처