반응 #2161227

반응 방정식

isobutyric acid chloride

(R)-2-[3-(diisopropylamino)-1-phenylpropyl]-4-(hydroxymethyl)phenol

→

Fesoterodine

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도cooling by ice bath
2. 2
   기타A white substance precipitated after approximately 5 minutes
3. 3
   workup.ADDITIONFor this purpose, drops of a solution of 17.7 g triethylamine in 250 ml dichloromethane were added in 5 minutes under agitation and ice bath
4. 4
   온도cooling
5. 5
   세척The batch was washed once with each of 250 ml water, 250 ml approximate 5% aqueous NaHCO3 solution and 250 ml water
6. 6
   추출The dichloromethane extract
7. 7
   건조dried over Na2SO4
8. 8
   기타was evaporated to a low small bulk on a rotary evaporator to constant weight, whereby a sallow, high viscosity oil
9. 9
   workup.WAITwas left

실험 절차

Drops of a solution of 18.6 g isobutyric acid chloride in 250 ml dichloromethane were added in approximately 10 minutes to a solution of 59.8 g (175.1 mol) (R)-2-[3-(diisopropylamino)-1-phenylpropyl]-4-(hydroxymethyl)phenol cooled to −3° C. (A, see FIG. 1) dissolved in 750 ml dichloromethane with agitation and cooling by ice bath. A white substance precipitated after approximately 5 minutes. For this purpose, drops of a solution of 17.7 g triethylamine in 250 ml dichloromethane were added in 5 minutes under agitation and ice bath cooling. The batch was washed once with each of 250 ml water, 250 ml approximate 5% aqueous NaHCO3 solution and 250 ml water. The dichloromethane extract dried over Na2SO4 was evaporated to a low small bulk on a rotary evaporator to constant weight, whereby a sallow, high viscosity oil was left.

출처