Methanol → (3,3-Dimethoxy-1-vinylcyclobutyl)methanol

To a solution of methyl 3,3-dimethoxy-1-vinylcyclobutanecarboxylate (2.02 g, 10.09 mmol) in THF (20 mL) was added DIBAL-H (1.04M in toluene, 29 mL, 30.16 mmol) at 0° C. under argon, and the mixture was stirred for 30 minutes at 0° C. To the mixture was carefully added MeOH (29 mL) and Na2SO4.10H2O (29 g), and the mixture was stirred overnight. The mixture was filtered and evaporated under reduced pressure. And the residue was diluted with hexane/EtOAc=1:1 and filtrated through the pad of silica gel and concentrated in vacuo to give (3,3-dimethoxy-1-vinylcyclobutyl)methanol (1.42 g).

1. stirringthe mixture was stirred overnight
2. filtrationThe mixture was filtered
3. customevaporated under reduced pressure
4. additionAnd the residue was diluted with hexane/EtOAc=1:1
5. filtrationfiltrated through the pad of silica gel
6. concentrationconcentrated in vacuo

ORD-Eintrag

ord-3de55fefbf3b4cda953173b8834f245d

Quelldatensatz

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09242973B2