反応 #1832012

反応方程式

product

4-{5-[2-(4-Benzo[d]isothiazol-3-yl-piperazin-1-yl)-ethyl]-6-chloro-2-oxo-2,3-dihydro-indol-1-yl}-4-oxo-butyric acid ethyl ester, hydrochloride salt

sodium hydrogen carbonate

→

4-{5-[2-(4-Benzo[d]isothiazol-3-yl-piperazin-1-yl)-ethyl]-6-chloro-2-oxo-2,3-dihydro-indol-1-yl}-4-oxo-butyric acid ethyl ester

溶媒

dichloromethane

Dichloromethane

反応条件

後処理

1. 1
   抽出The reaction mixture was extracted with dichloromethane (2×100 mL)
2. 2
   その他separated from the aqueous layer
3. 3
   洗浄the combined organic layer washed with water (4×200 mL)
4. 4
   乾燥The washed organic layer was dried over anhydrous sodium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮concentrated under vacuum to approximately 100 mL
7. 7
   濃縮To the concentrate thus obtained acetonitrile (500 mL)
8. 8
   workup.ADDITIONwas added
9. 9
   その他crystallization
10. 10
    workup.ADDITIONwas initiated during this addition
11. 11
    濃縮the resultant crystal slurry further concentrated under vacuum
12. 12
    その他to remove the remainder of the dichloromethane
13. 13
    ろ過This solid was filtrated
14. 14
    その他dried in a vacuum oven at 60° C.

実験手順

The product of example 1 or example 7 (15.0 g, 26.0 mmol), dichloromethane (150 mL) and 5% w/v aqueous sodium hydrogen carbonate solution (150 mL) were combined and the resultant mixture was well stirred for 25 min at 35° C. Dichloromethane (100 mL) was then added and stirring was continued for 20 min. at 30° C. The reaction mixture was extracted with dichloromethane (2×100 mL), separated from the aqueous layer and the combined organic layer washed with water (4×200 mL). The washed organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to approximately 100 mL. To the concentrate thus obtained acetonitrile (500 mL) was added, crystallization was initiated during this addition, and the resultant crystal slurry further concentrated under vacuum to remove the remainder of the dichloromethane. This solid was filtrated and dried in a vacuum oven at 60° C.

出典