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To a solution of crude pyrrolidine-3-carboxylic acid ethyl ester(7. 12 g) inCH2C12 (50 mL) at 0 C was added a solution of di-tert-butyl dicarbonate (10.30 g, 47.2 mmol) inCHzClz (50 mL) over 10 minutes. After warming to room temperature over 18 hours, the reaction mixture was washed with water, then brine, dried(Na2S04) and concentrated under reduced pressure to leave the title compound which was used without further purification (10.4 g, 100percentyield). 1H NMREI(CDCl3) 4.14 (q, 2H), 3.27-3. 69 (m, 4H), 3.02 (m, 1H), 2.07-2. 16 (m, 2H), 1.46 (s, 9H), 1.27 (t, 3H).
100%
at 0 - 20℃; for 18.1667 h;
To a solution of crude pyrrolidine-3-carboxylic acid ethyl ester (7.12 g) inCH2C12 (50mL) at0 C was added a solution of di-tert-butyl dicarbonate (10.30 g, 47.2 mmol) in CH2C12 (50 mL) over 10 minutes. After warming to room temperature over 18 hours, the reaction mixture was washed with water, then brine, dried(Na2S04) and concentrated under reduced pressure to leave the title compound which was used without further purification (10.4 g, 100percentyield). 1H NMR Cl (CDCl3) 4.14 (q, 2H), 3.27-3. 69 (m, 4H), 3.02 (m,1H), 2.07-2. 16 (m,2H), 1.46 (s,9H), 1.27 (t, 3H).
With hydrogenchloride; In 1,4-dioxane; dichloromethane; at 20℃; for 3.0h;
Step 2: hydrochloric acid/dioxane (30 mL) was slowly added in a dichloromethane solution (10 mL) of 1-t-butyloxycarbonyl-pyrrole-3-carboxylic acid ethyl ester (5.50 g, 22.61 mmol), and the reaction solution was stirred for 3 h at normal temperature. TLC showed that the reaction was completed. The mixture was concentrated under reduced pressure to obtain ethyl pyrrolidyl-3-carboxylate hydrochloride (4.00 g, crude product) which was buff oily matter. The product was directly used in next step without further purification. The value of C7H13NO2[M+H]+144 was calculated using MS ESI, and was 144.
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