반응 #1779369

반응 방정식

methanol

Trityl chloride

1-O-benzyl-(R)-glycerol

4-diethylaminopyridine

→

(R)-1-O-Benzyl-3-O-tritylglycerol

용매

pyridine

반응 조건

후처리

1. 1
   온도cooling with ice
2. 2
   workup.ADDITIONwas added
3. 3
   workup.STIRRINGthe mixture was stirred for 30 min
4. 4
   농축concentrated in vacuo to half of the original volume
5. 5
   workup.ADDITIONEthyl acetate (500 mL) was added
6. 6
   추출the mixture extracted with water (3×250 mL)
7. 7
   건조The organic layer was briefly dried with MgSO4
8. 8
   여과filtered
9. 9
   기타evaporated in vacuo
10. 10
    기타to remove the residual pyridine
11. 11
    기타used for further synthesis

실험 절차

Trityl chloride (56 g) was added portionswise to a solution of 1-O-benzyl-(R)-glycerol (36.4 g, 0.2 mol) and 4-diethylaminopyridine (1 g) in pyridine (300 mL) under stirring and cooling with ice. After 20 h stirring methanol (50 mL) was added, the mixture was stirred for 30 min and concentrated in vacuo to half of the original volume. Ethyl acetate (500 mL) was added and the mixture extracted with water (3×250 mL). The organic layer was briefly dried with MgSO4, filtered and evaporated in vacuo. The residue 4 was codistilled with toluene (200 ml portions) to remove the residual pyridine and used for further synthesis.

출처