反応 #44622

反応方程式

sodium hydrogencarbonate

hydrochloric acid ethyl acetate

(R)-2-tert-butoxycarbonylamino-5-(4-chlorophenyl)-5-oxopentanoic acid ethyl ester

→

title compound

収率 91.8%

(R)-5-(4-chlorophenyl)-3,4-dihydro-2H-pyrrole-2-carboxylic acid ethyl ester

収率 91.8%

溶媒

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   その他The resulting reaction solution
2. 2
   濃縮concentrated under reduced pressure
3. 3
   その他to give 5.0 g of a yellow oily substance
4. 4
   その他The resulting reaction solution
5. 5
   workup.STIRRINGwas stirred at room temperature for 20 min
6. 6
   抽出extracted with ethyl acetate
7. 7
   洗浄The extract solution was washed with saturated saline
8. 8
   乾燥dried over anhydrous magnesium sulfate
9. 9
   濃縮concentrated under reduced pressure

実験手順

A 4 N hydrochloric acid-ethyl acetate solution (30 mL) was dropwise added to an ethyl acetate solution (30 mL) of (R)-2-tert-butoxycarbonylamino-5-(4-chlorophenyl)-5-oxopentanoic acid ethyl ester (5.6 g) at room temperature. The resulting reaction solution was stirred at room temperature for 2 hr and concentrated under reduced pressure to give 5.0 g of a yellow oily substance. To an ethyl acetate solution (100 mL) of this crude product, a saturated sodium hydrogencarbonate aqueous solution (100 mL) was dropwise added. The resulting reaction solution was stirred at room temperature for 20 min and then extracted with ethyl acetate. The extract solution was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 3.5 g of the title compound as a light yellow oily substance. The physical property values of this compound were as follows:

出典