Formic Acid → (1-Methyl-3-piperidyl)methanol

A! At 0° C., 3-hydroxymethyl-piperidine (20 g, 173 mmoles) was slowly added to formic acid (63 ml, 1.66 moles) then a 40% solution of formaldehyde was added (62.4 ml, 833 mmoles). The mixture was refluxed for 5 hours, then the solvent was evaporated and the residue taken up in little water, brought to basic pH with 32% sodium hydroxide and extracted with ethyl ether. The organic phase was anhydrified over sodium sulfate and evaporated. The resultant crude was purified by distillation and provided 17 g (yield: 76%) of N-methyl-3-hydroxymethylpiperidine (b.p.--85°-86° C./1 mmHg).

1. temperatureThe mixture was refluxed for 5 hours
2. customthe solvent was evaporated
3. extractionextracted with ethyl ether
4. customevaporated
5. distillationThe resultant crude was purified by distillation

ORDレコード

ord-68a2ee096080469aa9ade94c557ef8e8

出典データセット

uspto-grants-1998_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05827881