Methanol → 3-methoxycarbonylcyclohexa-1,4-diene

Concentrated H2SO4 (1 ml) was added to a solution of 1,4-dihydrobenzoic acid (3 g, 23.97 mmol) in freshly dried methanol (10 ml). The reaction was heated to reflux in air for 1 h, cooled, poured into H2O (25 ml) and extracted with ether (3×50 ml). The combined ether layers were washed with 5% Na[HCO3] solution (50 ml) and saturated NaCl solution (50 ml) and dried over MgSO4. The ether was removed on the rotary evaporator to leave a colourless oil which was used without further purification.

1. temperatureThe reaction was heated
2. temperatureto reflux in air for 1 h
3. temperaturecooled
4. extractionextracted with ether (3×50 ml)
5. washThe combined ether layers were washed with 5% Na[HCO3] solution (50 ml) and saturated NaCl solution (50 ml)
6. dry with materialdried over MgSO4
7. customThe ether was removed on the rotary evaporator
8. customto leave a colourless oil which
9. customwas used without further purification

ORDレコード

ord-4b9adb23a35e42bebf946fb66ec1cf8a

出典データセット

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06750251B2