Diethyl Ether → HCID 15706331, compound

Temperature

0 °C

3.58 g (12.7 mmol) of the t-butoxycarbonyl protected precursor was added to a -10° C. cold mixture of 1.38 ml (12.7 mmol) of anisole and 40 ml of trifluoroacetic acid. After stirring for 30 minutes at 0° C., the solvent was removed in vacuo and the residue was stirred with dry ether, collected by suction and dried in vacuo over phosphorous pentoxide; yield: 3.77 g. 2.59 ml (14.0 mmol) of N-methyl-N-trimethylsilyltrifluoroacetamide was added to a suspension of 1.38 g (4.65 mmol) of this trifluoroacetic acid salt in 20 l of dry acetonitrile. After stirring for 30 minutes at room temperature, the mixture was evaporated in vacuo and the residue was taken up in a few ml of dry ether and 0.6 ml of methanol was added. The solution was evaporated again in vacuo and the residue was stirred with petroleum ether until the sticky material became crystalline; yield: 0.79 g.

1. customthe solvent was removed in vacuo
2. stirringthe residue was stirred with dry ether
3. customcollected by suction
4. dry with materialdried in vacuo over phosphorous pentoxide
5. stirringAfter stirring for 30 minutes at room temperature
6. customthe mixture was evaporated in vacuo
7. additionwas added
8. customThe solution was evaporated again in vacuo
9. stirringthe residue was stirred with petroleum ether until the sticky material

ORD record

ord-7436696894ed4699b4e4e59c61a93be5

Source dataset

uspto-grants-1989_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04801705