Reaktion #529760
ord-c973779e5d994e7f9e28e6e1ee5328ac
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONDuring the addition a white precipitate
- 2Sonstigewas formed
- 3Filtrationthe resultant voluminous white solid was filtered off
- 4Waschenwashed with water until acid-free and
- 5Trocknendried (phosphorus pentoxide) in vacuo
Vorschrift
Methyl chloroformate (12.90 g, 0.137 mol) was added dropwise, over 10 minutes, to a stirred, cooled (5° C.) solution of compound 3 (10.00 g, 0.047 mol) in sodium hydroxide (5.44 g, 0.136 mol) and water (150 ml). During the addition a white precipitate was formed and this stirred mixture was allowed to warm to room temperature overnight. The resultant mixture was carefully acidified (pH 5) with dilute hydrochloric acid and the resultant voluminous white solid was filtered off, washed with water until acid-free and dried (phosphorus pentoxide) in vacuo.