Ethyl 2-methyl-3,4-pentadienoate → ethyl (2E)-2-methylpenta-2,4-dienoate
反応式
[O-]CC.[Na+].[CH3:5][CH:6]([CH:12]=[C:13]=[CH2:14])[C:7]([O:9][CH2:10][CH3:11])=[O:8]>C(O)C>[CH3:5]/[C:6](=[CH:12]\[CH:13]=[CH2:14])/[C:7]([O:9][CH2:10][CH3:11])=[O:8]参加物
4
実験手順
Sodium ethoxide solution (21% in ethanol, 33.3 ml, cat.) was added to a solution of ethyl 2-methylpenta-3,4-dienoate (Bedoukian, 125.0 g, 890 mmol) in anhydrous ethanol (350 ml) and stirred at ambient temperature for 12 hours. The solution was concentrated in vacuo and the residue partitioned between ether and saturated NH4Cl solution. The aqueous phase was re-extracted twice with ether, then the combined organic phase washed with NH4Cl and then brine, dried over Na2SO4, filtered and the solvents removed in vacuo to yield the crude ester, 125.8 g as an orange oil which was used directly in the next step without further purification.
後処理
- concentrationThe solution was concentrated in vacuo
- customthe residue partitioned between ether and saturated NH4Cl solution
- extractionThe aqueous phase was re-extracted twice with ether
- washthe combined organic phase washed with NH4Cl
- dry with materialbrine, dried over Na2SO4
- filtrationfiltered
- customthe solvents removed in vacuo
出典と根拠
- ORDレコード
- ord-327c38d476ca44b78c732aec9b390698
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09156770B2
反応ノート
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