Reaktionsgleichung
O.[CH3:2][C@@:3]12[C:11](=[O:12])[CH2:10][CH2:9][C@H:8]1[C@@H:7]1[CH2:13][CH2:14][C:15]3[C@@H:21]([C@H:6]1[CH2:5][CH2:4]2)[CH2:20][CH2:19][C:17](=[O:18])[CH:16]=3.Cl[CH2:23][CH2:24]Cl>>[CH3:2][C@@:3]12[C@:11]([OH:12])([C:23]#[CH:24])[CH2:10][CH2:9][C@H:8]1[C@@H:7]1[CH2:13][CH2:14][C:15]3[C@@H:21]([C@H:6]1[CH2:5][CH2:4]2)[CH2:20][CH2:19][C:17](=[O:18])[CH:16]=3Komponenten
Versuchsvorschrift
A water-jacketed glass column of 2.7 cm inner diameter is packed with a suspension of 50.0 g of basic alumina (sold by Shokubai Kasei Kogyo Co. Ltd. under trade name of ACBR-3, calcined at a temperature above 500° C. and pulverized to about 50 mesh) in 100 ml of 1,2-dichloroethane (to a depth of 13.0 cm) and water is passed through the jacket so as to set the temperature at 20° C. In 1400 ml of 1,2-dichloroethane, 20.00 g of crude 19-norethisterone of 91.8% purity which results from ethynylation of 19-norandrost-4-ene-3,17-dione and which contains 1.7% ethynylestradiol in addition to other impurities is dissolved at 20° C. and the resulting solution is introduced on the top of the column at a linear velocity of 2 m/hr using a feed pump. The 1,2-dichloroethane solution passed through the alumina is received in an Erlenmeyer flask. After the solution of 19-norethisterone in 1,2-dichloroethan has been passed, 500 ml of 1,2-dichloroethane is further passed through the alumina to wash it. The two liquids are combined and concentrated to dryness at reduced pressure with 1,2-dichloroethane being distilled off.
Aufarbeitung
- customcalcined at a temperature above 500° C.
- customat 20° C
Quellen und Nachweise
- ORD-Eintrag
- ord-c3783980079b406792d0b7ba2a228691
- Quelldatensatz
- uspto-grants-1979_03
- Patentnummer
- US04144254
Verknüpfte Notizen
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