Reaktion #543542

Reaktionsgleichung

12-phthalimido-3,3,9,9-tetramethyl-5-oxa-4,8-diaza-2,10-dodecane dione dioxime

12-Phthalimido-3,3,9,9-tetramethyl-5-oxa-4,8-diaza-2,10-dodecanedione dioxime

hydrazine

→

12-Amino-3,3,9,9-tetramethyl-5-oxa-4,8-diaza-2,10-dodecanedione dioxime

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture was refluxed for 3 h
2. 2
   SonstigeThe white solid formed
3. 3
   Filtrationwas filtered
4. 4
   Waschenthe filter cake was washed with methylene chloride (50 mL)
5. 5
   EinengenThe combined filtrate and the washings were concentrated
6. 6
   Sonstigeto give a thick oil which
7. 7
   Sonstigewas dried under vacuum
8. 8
   Sonstigeto afford a white solid
9. 9
   SonstigeThis was used in the next step without further purification

Vorschrift

To a solution of 12-phthalimido-3,3,9,9-tetramethyl-5-oxa-4,8-diaza-2,10-dodecane dione dioxime (52a) (2.0 g, 4.6 mmol) in methylene chloride (100 mL) was added hydrazine (0.3 mL, 9.3 mmol) and the reaction mixture was refluxed for 3 h. The white solid formed was filtered and the filter cake was washed with methylene chloride (50 mL). The combined filtrate and the washings were concentrated to give a thick oil which was dried under vacuum to afford a white solid. Yield: 1.2 g (82%). MS: (M+H)+=304.1. This was used in the next step without further purification.

Quelle