Synthesis of Tris(2,6-dimethoxyphenyl)phosphine oxide

Yuichi Kitagawa; Satoshi Wada; M. D. Jahidul Islam; Kenichiro Saita; Masayuki Gon; Koji Fushimi; Kazuo Tanaka; Satoshi Maeda; Yasuchika Hasegawa

Improve Research Reproducibility A Bio-protocol resource

Home
Protocols

Concise Method

Synthesis of Tris(2,6-dimethoxyphenyl)phosphine oxide

YK Yuichi Kitagawa

SW Satoshi Wada

MI M. D. Jahidul Islam

KS Kenichiro Saita

MG Masayuki Gon

KF Koji Fushimi

KT Kazuo Tanaka

SM Satoshi Maeda

YH Yasuchika Hasegawa

This method is extracted from research article: Commun Chem, Aug 2020

Chiral lanthanide lumino-glass for a circularly polarized light security device

DOI: 10.1038/s42004-020-00366-1

Ask a question

Favorite

Tris(2,6-dimethoxyphenyl)phosphine (8.84 g, 0.02 mol) was dissolved in dichloromethane (30 mL) in a 100-mL flask, which was cooled in an ice bath. H₂O₂ solution (5 mL) was added slowly to the solution. The mixture was stirred for 3 h. The product was extracted with dichloromethane and saturated NaCl aqueous solution. The organic layer was dried with anhydrous MgSO₄, and the solvent was evaporated. The obtained oil was precipitated with acetone and hexane. The precipitate was filtered and washed with acetone to afford white powder.

Yield: 3.95 g (41%). δ/ppm = 7.23 (t, 3H, J = 8 Hz, Ar), 6.48 (dd, 6H, J = 8 and 4.8 Hz, Ar), 3.51 (s, 18H, CH₃). ESI-MS (m/z): [M+H]⁺ calculated for C₂₄H₂₈O₇P, 459.15; found, 459.16. Elemental analysis: Calcd for C₂₄H₂₇O₇P: C, 62.88%, H, 5.94%. Found: C, 62.55%, H, 5.88%.

Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this license, visit http://creativecommons.org/licenses/by/4.0/.

Do you have any questions about this protocol?

Post your question to gather feedback from the community. We will also invite the authors of this article to respond.

Post a Question

0 Q&A

Share your protocol with your peers.

Submit a Preprint Protocol