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HRID 42785作成日:2026年10月25日

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

https://huagongshe.com/reaction/42785

反応式

関与物質

役割名称HCID仕込み量
反応物NitrogenHCID 947—
反応物TriethylamineHCID 8471—
反応物Methanesulfonyl chlorideHCID 31297—
反応物[6-(2-Methyl-[1,3]dioxolan-2-yl)-pyridin-2-yl]-methanolHCID 66928639—
触媒4-(Dimethylamino)pyridineHCID 14284—
溶媒DichloromethaneHCID 6344—
生成物Methanesulfonic acid 6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-ylmethyl esterHCID 86649482—

反応条件

温度0 °C

反応手順

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.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08536209B2
出典データセットuspto-grants-2013_09
ORD IDord-4758c3e68a7d43f888e55d711618913e
出典メモuspto-grants-2013_09