Methanol → HCID 178495619, compound
Reaction equation
[CH3:1][OH:2].C[O-].[Na+].O.[C:7]1([CH3:13])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>>[CH3:1][O:2][CH2:13][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH2:9][CH2:8]1Participants
Procedure
Slices of metal Na (17.4 g, 0.755 mol) were added in small portions to methyl alcohol (250 ml) agitated at room temperature to prepare sodium methoxide. After metal Na pieces disappeared, a solution obtained by dissolving the compound (IV) (200.0 g, 0.581 mol) obtained above, in dry toluene (600 ml), was gradually added through a dropping funnel so that the inner temperature could keep within a range of 50° to 60° C. After completion of the addition, the mixture was refluxed for 4 hours, followed by cooling, adding water (20 ml), transferring into a separating funnel, washing the resulting toluene layer with water until the aqueous layer became neutral, distilling off toluene under reduced pressure, distilling under reduced pressure and collecting fractions of boiling points of 105°~108° C./1.5 mmHg to obtain trans-4-methyloxymethyl-1-phenylcyclohexane (V) (100.0 g).
Workup
- customa solution obtained
- additionwas gradually added through a dropping funnel so that the inner temperature
- customcould keep within a range of 50° to 60° C
- additionAfter completion of the addition
- temperaturethe mixture was refluxed for 4 hours
- temperatureby cooling
- customtransferring into a separating funnel
- washwashing the resulting toluene layer with water until the aqueous layer
- distillationdistilling off toluene under reduced pressure
- distillationdistilling under reduced pressure
- customcollecting fractions of boiling points of 105°~108° C./1.5 mmHg
Sources & evidence
- ORD record
- ord-46eedee3b1d04c73b6a791f3d37f7b79
- Source dataset
- uspto-grants-1986_10
- Patent number
- US04617141
Reaction notes
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