反応 #1242793

反応方程式

trans-4-(4-chlorophenoxy)-1-methyl-3-phenylpiperidine

potassium carbonate

ethyl chloroformate

→

trans-4-(4-chlorophenoxy)-1-ethoxycarbonyl-3-phenylpiperidine

溶媒

benzene

反応条件

後処理

1. 1
   温度is refluxed for 18 hours under nitrogen
2. 2
   その他The mixture is then partitioned
3. 3
   workup.DISTILLATIONbetween distilled water and hexane
4. 4
   洗浄The organic phase is washed with water
5. 5
   抽出the combined aqueous extracts are extracted with hexane
6. 6
   洗浄the combined organic extracts are washed with saturated aqueous NaCl solution
7. 7
   乾燥dried over anhydrous MgSO4
8. 8
   濃縮concentrated in vacuo
9. 9
   その他to afford an oil which
10. 10
    その他almost completely crystallizes
11. 11
    その他The colorless solid is triturated with hexane
12. 12
    ろ過filtered
13. 13
    洗浄washed well with hexane

実験手順

A mixture of 10.26 g of trans-4-(4-chlorophenoxy)-1-methyl-3-phenylpiperidine of Example 26, 7.05 g of anhydrous potassium carbonate, 75 ml of dry benzene and 5.53 g of ethyl chloroformate is refluxed for 18 hours under nitrogen. The mixture is then partitioned between distilled water and hexane. The organic phase is washed with water, the combined aqueous extracts are extracted with hexane, the combined organic extracts are washed with saturated aqueous NaCl solution, dried over anhydrous MgSO4, and concentrated in vacuo to afford an oil which almost completely crystallizes after standing for about 64 hours. The colorless solid is triturated with hexane, filtered and washed well with hexane to afford trans-4-(4-chlorophenoxy)-1-ethoxycarbonyl-3-phenylpiperidine, m.p. s 80°, 81.5°-84° C.

出典