Phenothiazine → Methallyl phosphonic acid diisopropyl ester

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Reaction Steps

208 parts of triisopropyl phosphite, 1.5 parts of phenothiazine and 3.4 parts of Ni(CO)4 (corresponding to 2 mol %, based on the phosphite) are heated to 120°-130° C in a nitrogen atmosphere. 99 parts (corresponding to a 10% excess) of methallyl chloride are added dropwise over a period of 5 hours. 68 parts of isopropyl chloride (Bp: 35°-36° C) are distilled off through a column. The product is fractionated in vacuo through a column. Boiling point: 58°-63° C/0.25 Torr; Yield: 155 parts (70.5% of the theoretical): nD20 : 1.4312 Purity according to GC: 97.3%

Provenance & Evidence