反応 #78146

反応方程式

1-chloro-4-(4-pyridylmethyl)phthalazine

3-aminophenol

→

title compound

1-(3-Hydroxyanilino)-4-(4-pyridylmethyl)phthalazine

溶媒

methanol

acetate

potassium carbonate

反応条件

後処理

1. 1
   温度After cooling to RT
2. 2
   ろ過filtration
3. 3
   洗浄washing of the filter residue with methanol
4. 4
   その他drying under HV (8 h, 130° C.)

実験手順

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.

出典