Magidson, O. Yu. published the artcileSynthesis of Phenadone, Safety of 2-Chloro-N,N-dimethylpropan-1-amine hydrochloride, the publication is Meditsinskaya Promyshlennost SSSR (1957), 11(No. 3), 25-8, database is CAplus.
The synthesis of Phenadone proceeds in 6 stages. CH2:CHCH2Cl (300 g.) with 600 g. tech. H2SO4 (d. 1.8-1.82) at 25-30° 1 hr. gives 319.3 g. MeCH(OH)CH2Cl (I). I (300 g.) is added to 546 g. 37% aqueous Me2NH and 300 g. 40% NaOH below 40°, the mixture stirred 30 min., 150 g. 40% NaOH added, the mixture kept 12 hrs., and the upper layer fractionated to give 183.8 g. MeCH(OH)CH2NMe2 (II), also prepared from propylene oxide and Me2NH. II (250 g.) is added dropwise to 380 g. SOCl2 and 730 g. of dry (ClCH2)2 during 1-1.5 hrs. at 30° and the mixture boiled 2 hrs. to give 338 g. MeCHClCH2NMe2.HCl (III). Ph2CHCN (60 g.), 46.6 g. powd. NaOH, and 69 g. III heated to 90-100°, kept at this temperature 7 hrs. with stirring, cooled, diluted with 50 cc. of H2O, and worked up gave 46 g. Ph2C(CN)CH2CHMeNMe2 (IV), m. 88-90°. IV (80 g.) in 70 cc. dry xylene is treated with EtMgBr (from 10 g. Mg and 50 g. EtBr), 55-60° 3 hrs. with stirring, kept 12 hrs., and acidified with 10% HCl, the ether distilled and the temperature raised to 115° to distil ether, xylene, and H2O. The crystals in the residue are filtered off and washed with acetone to yield 89 g. EtCOCPh2CH2CHMeNMe2.HBr (V.HBr), m. 224°; V, m. 77°; V.HCl (Phenadone), m. 229-31°.
Meditsinskaya Promyshlennost SSSR published new progress about 4584-49-0. 4584-49-0 belongs to chlorides-buliding-blocks, auxiliary class Chloride,Salt,Amine,Aliphatic hydrocarbon chain, name is 2-Chloro-N,N-dimethylpropan-1-amine hydrochloride, and the molecular formula is C5H13Cl2N, Safety of 2-Chloro-N,N-dimethylpropan-1-amine hydrochloride.
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