تفاعل #78146
ord-13dac9bc62b74569911d6cec94e6ece0
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةAfter cooling to RT
- 2ترشيحfiltration
- 3غسيلwashing of the filter residue with methanol
- 4أخرىdrying under HV (8 h, 130° C.)
الإجراء التجريبي
A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.491 g (4.5 mmol) 3-aminophenol is heated under nitrogen atmosphere for 1 h at 90° C. and for 3 h at 120° C. The reaction mixture is then taken up in a mixture of 30 ml acetate and 20 ml 20% aqueous potassium carbonate solution while stirring for about 4 h, and the filtration material is digested for 20 min in 20 ml of boiling methanol. After cooling to RT, filtration, washing of the filter residue with methanol, and drying under HV (8 h, 130° C.), title compound is obtained with a water content of 1.94%; m.p. 217-219° C.; ESI-MS: (M+H)+=329.