Sulfuric Acid → 3-[(Methoxycarbonyl)methylthio]-2,6-dimethyl-4-heptanone
Reaction equation
OS(O)(=O)=O.C[O-].[Na+].[SH:9][CH:10]([C:14](=[O:19])[CH2:15][CH:16]([CH3:18])[CH3:17])[CH:11]([CH3:13])[CH3:12].[CH3:20][O:21][C:22](=[O:25])[CH2:23]Cl>CO.O>[CH3:20][O:21][C:22]([CH2:23][S:9][CH:10]([C:14](=[O:19])[CH2:15][CH:16]([CH3:18])[CH3:17])[CH:11]([CH3:13])[CH3:12])=[O:25]Participants
Conditions
- Temperature
- 24 °C
Procedure
Into a 50 ml, round-bottom, three-necked flask equipped with magnetic stirrer, pot thermometer, "Y" tube, nitrogen inlet tube, reflux condenser with cotton plug, H2SO4 bubbler for nitrogen, and cold water bath is added a solution of 0.65 grams of sodium methoxide dissolved in 10 ml anhydrous methanol. At a reaction mass temperature of 25°-28° C and over a period of one minute, with stirring, is added a solution of 2.1 grams of 3-mercapto-2,6-dimethyl-4-heptanone dissolved in 2 ml anhydrous methanol. After stirring 8 minutes, 1.30 grams of methylchloroacetate (0.012 moles) is added over a period of 2 minutes to the reaction mass; the temperature of the reaction mass rising to 38° C. The reaction mass is allowed to cool to 24° C and is stirred for a period of 2 hours.
Workup
- customInto a 50 ml, round-bottom, three-necked flask equipped with magnetic stirrer
- stirringAfter stirring 8 minutes
- customrising to 38° C
- stirringis stirred for a period of 2 hours
Sources & evidence
- ORD record
- ord-5b8974a000ec4ec786a76b23dcd0d374
- Source dataset
- uspto-grants-1978_04
- Patent number
- US04083862
Reaction notes
Loading…