반응 #7073

반응 방정식

triethyl amine

2-(4-Hydroxyphenyl)ethanol

Methanesulfonyl chloride

→

1-(Methylsulfonyloxy)-2-[4-(methylsulfonyloxy)phenyl]ethane

용매

methylene chloride

반응 조건

후처리

1. 1
   기타the temperature between −25° C. and −15° C
2. 2
   기타were formed which
3. 3
   여과were filtered off
4. 4
   세척washed with methylene chloride (600 ml)
5. 5
   세척The organic layer was washed first with saturated sodium hydrogencarbonate solution (700 ml) at 20° C.
6. 6
   기타The methylene chloride was evaporated to dryness

실험 절차

2-(4-Hydroxyphenyl)ethanol(356 g, 2.58 mol, 1.0 eq) was dissolved in methylene chloride (3500 ml) and triethyl amine (653 g, 6.44 mol, 2.5 eq). The mixture was cooled to −20° C. Methanesulfonyl chloride (657 g, 5.74 mol. 2.2 eq) was then added keeping the temperature between −25° C. and −15° C. When the conversion was >95% salts were formed which were filtered off and washed with methylene chloride (600 ml). The organic layer was washed first with saturated sodium hydrogencarbonate solution (700 ml) at 20° C. followed by water (700 ml). The methylene chloride was evaporated to dryness and the remaining residue was then used in the subsequent step.

출처