반응 #938206

반응 방정식

acetyl chloride

cis-4-(4-aminophenoxy)-1-methyl-3-phenylpiperidine

cis-4-(4-aminophenoxy)-1-methyl-3-phenylpiperidine dihydrochloride

triethylamine

→

cis-4-(4-acetamidophenoxy)-1-methyl-3-phenylpiperidine

용매

chloroform

chloroform

반응 조건

후처리

1. 1
   기타a maximum of 28° C
2. 2
   세척The chloroform solution is washed with 10% aqueous NaOH solution
3. 3
   건조with saturated aqueous NaCl solution, dried over anhydrous Na2SO4
4. 4
   농축concentrated in vacuo to a foam which
5. 5
   온도The hexane mixture is briefly heated
6. 6
   workup.WAITto stand for 30 minutes
7. 7
   여과before filtering
8. 8
   기타A crude solid results
9. 9
   기타s 172°, 173°-175° C
10. 10
    기타Recrystallization from toluene

실험 절차

A solution of 1.4 ml of acetyl chloride in 75 ml of chloroform is added dropwise under nitrogen over a 15-minute period to a solution of 5.05 g of the free base of cis-4-(4-aminophenoxy)-1-methyl-3-phenylpiperidine of Example 8 in 150 ml of dry chloroform containing 2.74 ml of triethylamine. The pot temperature reaches a maximum of 28° C. The reaction is complete in 30 minutes. The chloroform solution is washed with 10% aqueous NaOH solution, then with saturated aqueous NaCl solution, dried over anhydrous Na2SO4 and concentrated in vacuo to a foam which solidifies upon trituration with hexane. The hexane mixture is briefly heated to boiling, then cooled to room temperature and allowed to stand for 30 minutes before filtering. A crude solid results, mp s 172°, 173°-175° C. Recrystallization from toluene affords cis-4-(4-acetamidophenoxy)-1-methyl-3-phenylpiperidine, mp 174.5°-176.5° C.

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