2-METHYL-2-HEPTANOL synthesis
- Product Name:2-METHYL-2-HEPTANOL
- CAS Number:625-25-2
- Molecular formula:C8H18O
- Molecular Weight:130.23
Yield:-
Reaction Conditions:
in diethyl ether for 6 h;Inert atmosphere;Cooling with ice;
Steps:
1 EXAMPLE 1: Preparation of 2-hydroxy-2-methylheptane from ethyl caproate
To an oven-dried 2L three-neck round bottom flask equipped with a condenser,an addition funnel, and an inlet adapter was charged 800ml of a 3M solution (2.4mol) ofmethylmagnesium bromide in diethylether via cannula under a nitrogen atmosphere. Tothe addition funnel was added a solution of I50g (I. 04mol) of ethyl caproate in I OOmL15 of anhydrous ether. The round bottom was immersed into an ice bath and the solution inthe addition funnel was added dropwise over a period of 2 hours. After the addition wascomplete, the ice bath was removed and the solution was allowed to stir for an additional4 hours until the reaction was complete. The round bottom was immersed into an icebath once again and the reaction quenched by dropwise addition of IN HCl until the20 evolution of gas ceased. At this point IN HCl was added at a faster rate until all solidsdissolved and the organic layer became clear and yellow. The mixture was transferred toa separatory funnel and the bottom aqueous layer was removed. The organic layer wasthen washed with 3 x 500ml of IN HCl. The aqueous washes were then combined andreextracted with 500ml of diethylether. The combined organic layers were then washed25 with water and brine and the solvent carefully removed on a rotary evaporator to affordI27.85g of crude 2-hydroxy-2-methylheptane as a yellow oil
References:
TAKASAGO INTERNATIONAL CORPORATION (USA);LOMBARDO, Louis, J.;LANKIN, Michael, E.;DEROSA, Frank WO2017/214446, 2017, A1 Location in patent:Page/Page column 21
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