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HRID 1929301作成日:2026年10月27日

Triethylamine → 4-Ethynylbenzyl methanesulfonate

https://huagongshe.com/reaction/1929301

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Methanesulfonyl chlorideHCID 31297—
反応物(4-Ethynylphenyl)methanolHCID 11170993—
溶媒DichloromethaneHCID 6344—
生成物4-Ethynylbenzyl methanesulfonateHCID 5943577388.1%

反応手順

To a solution of 4-ethynylbenzyl alcohol (5.0 g, 37.8 mmol) in CH2Cl2 (50 mL) and triethylamine (Et3N) (14.4 mL, 104.0 mmol) was added mesyl chloride (8.04 mL, 104.0 mmol) at 0° C. and the reaction was allowed to warm to room temperature. Stirring continued for 2 h under argon during which TLC revealed a quantitative conversion into a higher Rf product. Ice cold water was added into the reaction mixture and extracted with Et2O (200 ml). The organic layer was washed with 1N HCL (70 ml), H2O (100 ml), aqueous NaHCO3 (70 ml), and finally H2O (100 ml); and then dried over Na2SO4. Solvent was evaporated off and dried in vacuo to give 7.0 g of compound 3 as brownish oil which was used without further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08188054B2
出典データセットuspto-grants-2012_05
ORD IDord-9b05b4722aaf48edbf4f4439c833e9fa
出典メモuspto-grants-2012_05