Method of preparing formaldoxime trimer

Organic compounds -- part of the class 532-570 series – Organic compounds – Four or more ring nitrogens in the bicyclo ring system

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544215, C07D25106

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active

046803947

ABSTRACT:
An improved process for preparing formaldoxime trimer is provided in which loss of the product is minimized and the prior art problems of long retention times to afford precipitation of the trimer which is difficult to filter and which occludes the undesirable salt of the acid that is difficult to remove. The method disclosed involved oximation of paraformaldehyde using dehydroxylamine sulfate and ammonia gas followed by steam stripping to recover formaldoxime and separate trimerization thereof followed by filtration recovery and drying.
The formaldoxime trimer is produced in essentially quantitative yield and proceeds specifically by a procedure of steam stripping out the formaldoxime monomer from the synthesis liquor and allowing separate trimer formation and recovery. The product is free from inorganic salts and the mother liquor with formaldoxime monomer content, resulting from its recovery by filtration, does not represent a yield loss in that it is recyclable to the next synthesis reaction.

REFERENCES:
patent: 4096187 (1978-06-01), Bonfield et al.
patent: 4155933 (1979-05-01), Bonfield et al.
patent: 4323706 (1982-04-01), Bonfield et al.
Mitsubishi Gas Chemical Company, CA, vol. 98, 1983, 98:127089q.
Funaoka et al, CA, vol. 75, 1971, 75: 153143x.
K. A. Jensen, et al. Invest. of Formaldehyde Oximes, Its Polymers and Coord. Cpds. I, Mat. Fys. Med, 40:1, pp. 3-23, (1978).
F. A. Anderson, et al., Invest. of Formaldehyde Oximes, Its Polymers and Coord. Cpds. II, Mat. Fys. Med. 40:2 pp. 3-24 (1978).

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