Process for the separation of 2,4-dinitro-6-t-butyl-3-methylanis

Details Process for the separation of 2,4-dinitro-6-t-butyl-3-methylanis Process for the separation of 2,4-dinitro-6-t-butyl-3-methylanis

1978-12-18

1980-11-11

Helfin, Bernard

Organic compounds -- part of the class 532-570 series

Organic compounds

Oxygen containing

C07C 7935

Patent

active

042334632

ABSTRACT:
The invention relates to a process for the separation of 2,4-dinitro-6-t-butyl-3-methylanisole, referred to as musk ambrette, from the crude mixtures in which it is present, which are obtained by nitrating 6-t-butyl-3-methylanisole.
According to the invention, an amount of water representing from 5 to 40% by weight of the nitrating mixture used in the synthesis is introduced onto the crude synthesis mixture in a first addition, the pure musk ambrette obtained is collected and several small amounts of water, representing from 1 to 15% by weight of the said nitrating mixture used, are then introduced, the precipitated product being collected between each addition. The process makes it possible to collect, in a pure form and without the use of an organic extraction solvent, about three quarters of the musk ambrette present in the crude synthesis mixture.

REFERENCES:
patent: 481685 (1892-08-01), Bauer
patent: 1875916 (1932-09-01), Clemmenson
patent: 1926080 (1933-09-01), Borman
patent: 2007234 (1935-07-01), Wirth
patent: 2476815 (1949-07-01), Carpenter et al.
patent: 2493797 (1950-01-01), Wood
Carpenter et al., Jour. of Org. Chemistry, vol. 16, (1951), 586-620.

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