反応 #66305

ord-95a9a672e4e74bd9b0b2f18826c1a00a

反応方程式

CC1(C)OB(c2ccc(C(=O)O)cc2)OC1(C)C
4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoic acid
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOCCl
chloromethyl ethyl ether
CCOCOC(=O)c1ccc(B2OC(C)(C)C(C)(C)O2)cc1
ethoxymethyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate
収率 84.0%

反応条件

温度
65°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    ろ過filtered
  3. 3
    濃縮the filtrate concentrated

実験手順

4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoic acid (0.50 g, 2.02 mmol) was dissolved in 20 mls of dry acetonitrile. To this solution was added powdered potassium carbonate (0.42 g, 3.02 mmol) followed by chloromethyl ethyl ether (0.24 mls, 2.42 mmol). This mixture was warmed to 65° C. for 2 hours, then allowed to cool to room temperature, filtered and the filtrate concentrated to give ethoxymethyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate as a solid (84%). This material was taken onto the next step without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524702B2uspto-grants-2013_09