반응 #71063

반응 방정식

Ms-Cl

N2

[6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-yl]-methanol

Et3N

→

title compound

Methanesulfonic acid 6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-ylmethyl ester

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타the reaction mixture was quenched with water (10 mL)
2. 2
   추출extracted with CH2Cl2 (10 mL)
3. 3
   건조extracts were dried over Na2SO4
4. 4
   여과filtered
5. 5
   기타the solvents were removed under reduced pressure
6. 6
   기타Purification of the residue by FC (70:30 to 50:50 hept-EA)

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-yl]-methanol (729 mg, 3.74 mmol) in dry CH2Cl2 (10.0 mL) was treated at 0° C. with Et3N (0.67 mL, 4.83 mmol) followed by DMAP (46 mg, 0.37 mmol) and Ms-Cl (0.37 mL, 4.72 mmol). After stirring at 0° C. for 1 h, the reaction mixture was quenched with water (10 mL), extracted with CH2Cl2 (10 mL) and the combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (70:30 to 50:50 hept-EA) gave the title compound as a pale yellow oil. LC-MS-conditions 02: tR=0.79 min; [M+H]+=274.39.

출처