Synlett 2020; 31(20): 2039-2042
DOI: 10.1055/s-0040-1706298
letter

Practical Transition-Metal-Free Protodeboronation of Arylboronic Acids in Aqueous Sodium Hypochlorite

Minxin Li
,
Yanling Tang
,
Jinchun Gao
,
Gaoxiong Rao
,
Zewei Mao
College of Pharmaceutical Science, Yunnan University of Chinese Medicine, Kunming 650500, P. R. of China   Email: maozw@ynutcm.edu.cn   Email: ydmason@163.com
› Author Affiliations
This work was financially supported by the Yunnan Provincial Science and Technology Department-Applied Basic Research Joint Special Funds of Yunnan University of Chinese Medicine [2017FF117(-023)].


Abstract

A concise and practical method was developed for the protodeboronation of arylboronic acids under mild conditions in aqueous NaClO at 100 °C. The strategy is low-cost, transition-metal-free, and base-free.

Supporting Information



Publication History

Received: 03 August 2020

Accepted after revision: 26 August 2020

Article published online:
07 October 2020

© 2020. Thieme. All rights reserved

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  • 14 Protodeboronation of Arylboronic Acids; General Procedure A solution of the appropriate arylboronic acid (1 mmol) and TBAB (64 mg, 0.2 mmol) in 10.5 wt% aq NaClO was stirred at 100 °C for 6–12 h until the reaction was complete (TLC). The mixture was extracted with Et2O (2 × 5 mL), and the organic layer was dried (Na2SO4) and concentrated in vacuo. The residue was purified by column chromatography [silica gel, PE–EtOAc (40:1 to 20:1)]. 1,4-Dimethoxybenzene (2a) Prepared from 1a according to the general procedure as a white solid; yield: 121 mg (88%); mp 51–53 °C. 1H NMR (400 MHz, CDCl3): δ = 6.86 (s, 4 H), 3.78 (s, 6 H).