Alkylphosphonyl dichlorides

The aluminum chloride process 2-3 is a general method for the preparation of alkylphosphonyl dichlorides. The procedure described here is essentially that of Kennard and Hamilton 4 and is based on the procedure of Kinnear and Perren.2... 

Alkylphosphonyl dichlorides, 37, 84 Alloxan monohydrate, 33, 3 Alloxan monohydrate, 32, 6 Alloxantin dihydrate, 33, 3 Allylbenzene, 31, 85, 86 Allylbromide, 31, 86, 36, 61 a Allyl 0 bromoethyl ethyl ether, 36, 62... 

Patois. C., Berte-Verrando, S., and Savignac, P., Easy preparation of alkylphosphonyl dichlorides. Bull. Soc. Chim. Fr., 130, 485, 1993. 

Bhongle, N.N., Notter, R.H., and Turcotte, J.G., Expedient and high-yield synthesis of alkylphosphonyl dichlorides under mild, neutral conditions. Reaction of f>w(trimethylsilyl)alkyl phosphonates with oxalyl chloride/dimethylformamide, Synth. Commun., 17, 1071, 1987. 

All Schedule 2 chemicals are analyzable by NMR, except arsenic trichloride, which does not possess a useful nucleus. Either an organic solvent or D20 is used. Note that the hydrolysis products of alkylphosphonofluoridates (l.A.l), alkylphos-phonothiolates (1.A.3), alkylphosphonyl difluorides (1.B.9), alkylphosphonites (1.B.10), chlorosarin (l.B.ll), and chlorosoman (1.B.12), which have an alkyl group (Me, Et, n-Pr, or i-Pr) finked direefly to a phosphorus, all belong to Schedule 2, group B.4, and NMR analysis for them is made either in D20 or in an organic solvent. By way of example, NMR spectral parameters of isopropyl methylphosphonate, pinacolyl methylphosphonate, methylphosphonic acid, 0-ethyl methylthiophos-phonate, N,N-dimethylphosphoramidic dichloride,... 

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