Fast and scalable solvent-free access to Lappert's heavier tetrylenes E{N(SiMe3)2}2 (E = Ge, Sn, Pb) and ECl{N(SiMe3)2} (E = Ge, Sn)

Javier A. Cabeza; Javier F. Reynes; Felipe García; Pablo García-Álvarez; Rubén García-Soriano

doi:10.1039/d3sc02709k

Fast and scalable solvent-free access to Lappert's heavier tetrylenes E{N(SiMe₃)₂}₂ (E = Ge, Sn, Pb) and ECl{N(SiMe₃)₂} (E = Ge, Sn)

Javier A. Cabeza
, Javier F. Reynes
, Felipe García
, Pablo García-Álvarez
, Rubén García-Soriano

School of Chemistry

Research output: Contribution to journal › Article › Research › peer-review

18 Citations (Scopus)

Abstract

Iconic Lappert's heavier tetrylenes E{N(SiMe₃)₂}₂ (E = Ge (1), Sn (2), Pb (3)) have been efficiently prepared from GeCl₂·(1,4-dioxane), SnCl₂ or PbCl₂ and Li{N(SiMe₃)₂} via a completely solvent-free one-pot mechanochemical route followed by sublimation. This fast, high-yielding and scalable approach (2 has been prepared in a 100 mmol scale), which involves a small environmental footprint, represents a remarkable improvement over any synthetic route reported over the last five decades, being a so far rare example of the use of mechanochemistry in the realm of main group chemistry. This solventless route has been successfully extended to the preparation of other heavier tetrylenes, such as ECl{N(SiMe₃)₂} (E = Ge (4), Sn (5)).

Original language	English
Pages (from-to)	12477-12483
Number of pages	7
Journal	Chemical Science
Volume	14
Issue number	44
DOIs	https://doi.org/10.1039/d3sc02709k
Publication status	Published - 28 Nov 2023

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SDG 12 Responsible Consumption and Production

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10.1039/d3sc02709kLicence: CC BY-NC

Cite this

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title = "Fast and scalable solvent-free access to Lappert's heavier tetrylenes E\{N(SiMe3)2\}2 (E = Ge, Sn, Pb) and ECl\{N(SiMe3)2\} (E = Ge, Sn)",

abstract = "Iconic Lappert's heavier tetrylenes E\{N(SiMe3)2\}2 (E = Ge (1), Sn (2), Pb (3)) have been efficiently prepared from GeCl2·(1,4-dioxane), SnCl2 or PbCl2 and Li\{N(SiMe3)2\} via a completely solvent-free one-pot mechanochemical route followed by sublimation. This fast, high-yielding and scalable approach (2 has been prepared in a 100 mmol scale), which involves a small environmental footprint, represents a remarkable improvement over any synthetic route reported over the last five decades, being a so far rare example of the use of mechanochemistry in the realm of main group chemistry. This solventless route has been successfully extended to the preparation of other heavier tetrylenes, such as ECl\{N(SiMe3)2\} (E = Ge (4), Sn (5)).",

author = "Cabeza, \{Javier A.\} and Reynes, \{Javier F.\} and Felipe Garc{\'i}a and Pablo Garc{\'i}a-{\'A}lvarez and Rub{\'e}n Garc{\'i}a-Soriano",

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T1 - Fast and scalable solvent-free access to Lappert's heavier tetrylenes E{N(SiMe3)2}2 (E = Ge, Sn, Pb) and ECl{N(SiMe3)2} (E = Ge, Sn)

AU - Cabeza, Javier A.

AU - Reynes, Javier F.

AU - García, Felipe

AU - García-Álvarez, Pablo

AU - García-Soriano, Rubén

PY - 2023/11/28

Y1 - 2023/11/28

N2 - Iconic Lappert's heavier tetrylenes E{N(SiMe3)2}2 (E = Ge (1), Sn (2), Pb (3)) have been efficiently prepared from GeCl2·(1,4-dioxane), SnCl2 or PbCl2 and Li{N(SiMe3)2} via a completely solvent-free one-pot mechanochemical route followed by sublimation. This fast, high-yielding and scalable approach (2 has been prepared in a 100 mmol scale), which involves a small environmental footprint, represents a remarkable improvement over any synthetic route reported over the last five decades, being a so far rare example of the use of mechanochemistry in the realm of main group chemistry. This solventless route has been successfully extended to the preparation of other heavier tetrylenes, such as ECl{N(SiMe3)2} (E = Ge (4), Sn (5)).

AB - Iconic Lappert's heavier tetrylenes E{N(SiMe3)2}2 (E = Ge (1), Sn (2), Pb (3)) have been efficiently prepared from GeCl2·(1,4-dioxane), SnCl2 or PbCl2 and Li{N(SiMe3)2} via a completely solvent-free one-pot mechanochemical route followed by sublimation. This fast, high-yielding and scalable approach (2 has been prepared in a 100 mmol scale), which involves a small environmental footprint, represents a remarkable improvement over any synthetic route reported over the last five decades, being a so far rare example of the use of mechanochemistry in the realm of main group chemistry. This solventless route has been successfully extended to the preparation of other heavier tetrylenes, such as ECl{N(SiMe3)2} (E = Ge (4), Sn (5)).

UR - https://www.scopus.com/pages/publications/85175164316

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DO - 10.1039/d3sc02709k

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