Reaktionsgleichung
[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[CH:7][N:8]=[N:9][C:10]=2[NH:11][NH2:12])[CH:6]=1.[ClH:13]>>[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[CH:7][N:8]=[N:9][C:10]=2[NH:11][NH2:12])[CH:6]=1.[ClH:13]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
Again according to the disclosure in the '397 application, hydralazine free base 25 g (1 part by weight) was heated in 165 mL (6 to 7 parts by volume) of 15% hydrochloric acid to a temperature of 70-80° C. The solution was filtered hot to remove traces of insoluble materials that were undesired by-products of the preceding step. One hundred sixty five milliliters of ethanol (6 to 7 parts by volume) was added to the filtrate. As the resulting solution cooled to 25° C. (ambient temperature) and then further cooled to 3-8° C., a pale yellow precipitate of the desired product, hydralazine hydrochloride, solidified. The obtained yield is 65% (the reported yields in the '397 application were 80-90%).
Aufarbeitung
- filtrationThe solution was filtered hot
- customto remove traces of insoluble materials that
- additionOne hundred sixty five milliliters of ethanol (6 to 7 parts by volume) was added to the filtrate
- temperaturefurther cooled to 3-8° C.
- customThe obtained yield is 65% (the reported yields in the '397 application
Quellen und Nachweise
- ORD-Eintrag
- ord-7f379bf022104df0a431a1e2088bf4aa
- Quelldatensatz
- uspto-grants-2010_10
- Patentnummer
- US07807830B2
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