Triethylamine → HCID 18381660, compound

Participants

Reaction Steps

4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-1-phenyl-1,2-dihydro-phthalazine (0.16 g, 0.4 mmole), prepared as described in example 111, in dry CH2Cl2 (10 ml), under N2, was added with triethylamine (0.1 ml, 0.72 mmole) and methanesulphonyl chloride (0.037 ml, 0.48 mmole). The mixture was stirred at room temperature overnight, then added again with triethylamine (0.05 ml, 0.36 mmole) and methanesulphonyl chloride (0.02 ml, 0.24 mmole). After 4 hours methanesulphonyl chloride (0.04 ml, 0.48 mmole) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.085 ml, 0.56 mmole) were added. After 24 hours the mixture was poured into water and the aqueous phase separated and extracted with CH2Cl2. The organic phase was washed in diluted citric acid, anhydrified and dried to give a solid which was flash chromatographed (eluent: petrolatum/ethyl acetate 7:3). The resultant solid was triturated in ethyl ether to give 0.21 g of the title compound (quantitative yield). m.p.: 222.6-224.4° C.

Provenance & Evidence