Hydrazine hydrate (1:1) → HCID 178423887、化合物

To a solution of 2-[(dimethylamino)methylene]-5,5-dimethylcyclopentanone (12.5 g, 75 mmol) in ethanol (100 mL) at room temperature was added hydrazine hydrate (4 mL, 82.3 mmol). The reaction mixture was heated at reflux overnight. It was then cooled to room temperature and concentrated. Water (700 mL) was added to the residue, and the resulting solution was extracted twice with diethyl ether (2×250 mL). The organic extracts were combined, dried over MgSO4 and concentrated to give the title compound as an oil (10.5 g). 1H NMR indicated the oil to be ˜60% pure. It was used directly for Step C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. concentrationconcentrated
4. additionWater (700 mL) was added to the residue
5. extractionthe resulting solution was extracted twice with diethyl ether (2×250 mL)
6. dry with materialdried over MgSO4
7. concentrationconcentrated

ORDレコード

ord-f657392d3ec74be3a5f9a13e2dda1db6

出典データセット

uspto-grants-2006_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07138361B2