反応 #8942

反応方程式

4-benzylpiperazine

NEt3

ethyl acetate hexane

benzyl 3-chlorosulfonyl-2(R)-methylpropionate

→

pure product

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

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet
2. 2
   濃縮then concentrated in vacuo
3. 3
   その他partitioned between ethyl acetate and saturated sodium bicarbonate
4. 4
   洗浄The combined organics were washed with brine
5. 5
   乾燥dried over Na2SO4
6. 6
   濃縮concentrated in vacuo
7. 7
   その他to yield 3.4 g crude product

実験手順

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.

出典