Acetic Acid → 2,6,6-Trimethylfulvene

To 130 ml of dehydrated methanol, 22.6 g (283 mmol) of methylcyclopentadiene and 8.50 ml (116 mmol) of acetone were added, then 14.5 ml (174 mmol) of pyrrolidine was dropwise added at 0° C., and the mixture was reacted at room temperature for one night. Then, 10 ml (180 mmol) of acetic acid was added at 0° C. The mixture was diluted with ether and water and then subjected to extraction. Then, the organic phase was separated, washed with water and dried over anhydrous magnesium sulfate to obtain 12.9 g of a brown liquid. The analyzed values are given below.

1. customthe mixture was reacted at room temperature for one night
2. extractionsubjected to extraction
3. customThen, the organic phase was separated
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate

ORD record

ord-02e1cd6f9c1b4900b49a714d7d59086e

Source dataset

uspto-grants-2008_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07449533B2