반응 #71026

반응 방정식

N2

[5-(2-methyl-[1,3]dioxolan-2-yl)-furan-2-yl]-methanol

Et3N

CH2Cl2

→

title compound

2-(5-Chloromethyl-furan-2-yl)-2-methyl-[1,3]dioxolane

반응 조건

후처리

1. 1
   기타the reaction mixture was quenched with water (40 mL)
2. 2
   추출extracted with CH2Cl2 (40 mL)
3. 3
   건조extracts were dried over MgSO4
4. 4
   여과filtered
5. 5
   기타the solvents were removed
6. 6
   기타Purification of the residue by FC (8:2:0.1 hept-EA-Et3N)

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [5-(2-methyl-[1,3]dioxolan-2-yl)-furan-2-yl]-methanol (3.50 g, 19.00 mmol) in dry CH2Cl2 (35.0 mL) was treated at 0° C. with Et3N (3.44 mL, 22.80 mmol) followed by DMAP (232 mg, 1.90 mmol) and Ms-C1 (1.77 mL, 22.80 mmol). After stirring at rt for 2 h, the reaction mixture was quenched with water (40 mL), extracted with CH2Cl2 (40 mL) and the combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced. Purification of the residue by FC (8:2:0.1 hept-EA-Et3N) gave the title compound as a yellow oil: TLC:rf (4:1 hept-EA)=0.35.

출처