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ChemicalBook CAS DataBase List CHEMBRDG-BB 4015569
59857-88-4

CHEMBRDG-BB 4015569 synthesis

1synthesis methods
-

Yield:-

Reaction Conditions:

in ethanol;nickel;benzene;

Steps:

2 2.

2. 4-Hydroxymethyl-1-isopropyl-pyrrolidone (III) 92.5 g (0.5 mol) of 4-carbomethoxy-1-isopropyl-pyrrolidone in 1.2 l of ethanol were hydrogenated in the presence of about 50 g of Raney-Nickel for 48 hours at 160° - 180° C under a hydrogen pressure of 200 atmospheres. Then it was determined with the aid of thin layer chromatography (CHCl3 /C2 H5 OH= 95:5) if the reduction was finished. Otherwise 20 g of Raney-Nickel were added again and hydrogenated for another 24 hours. In most of the tests hydrogenation had finished after this time. The catalyst was filtered with exclusion of air, the filtrate was concentrated in vacuo, the residue was mixed with 500ml of benzene and concentrated again. The product was then distilled over a Vigreux column having a 30 cm length. boiling point: 152° C/0.08 mm Hg; melting point: 45° C.

References:

US4071530,1978,A

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