Hydrochloric Acid → HCID 68798704, compound

Temperature

0 °C

To a suspension of Mg (2 g, 82.2 mmol) in dry ether (100 mL) was added CH3I (5 mL, 80.4 mmol) in dry ether (100 mL). After the addition was completed, the reaction mixture was refluxed for 1 hour and then cooled to 0° C. LiBH4 (2.0M in THF, 25 mL, 50 mmol) was added followed by addition of methyl 3,5-dimethoxy-4-i-propylbenzoate (10.0 g, 42.0 mmol) in dry ether (300 mL). The reaction was stirred at 0° C. overnight. Water (50 mL) was added dropwise followed by 2N HCl (100 mL). The organic layer was separated and the aqueous extracted with ether (4×200 mL). The extract was dried over anhydrous sodium sulfate. Evaporation of the solution yielded a liquid mixture. This was used directly in the next step without purification.

1. additionAfter the addition
2. temperaturethe reaction mixture was refluxed for 1 hour
3. customThe organic layer was separated
4. extractionthe aqueous extracted with ether (4×200 mL)
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. customEvaporation of the solution
7. customyielded a liquid mixture
8. customThis was used directly in the next step without purification

ORD record

ord-3af56e9bf53b470c8b277fba911d8f73

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08487009B2