تفاعل #1265398

معادلة التفاعل

2-amino-6-chloro-4-n-pentyloxypteridine

tri-o-tolylphosphane

styrene

triethylamine

→

orange powder

المردود 72.9%

2-amino-4-n-pentyloxy-6-styrylpteridine

المردود 72.9%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 90 hours
2. 2
   أخرىIt was evaporated
3. 3
   أخرىthe residue purified by silica gel column chromatography with chloroform
4. 4
   أخرىThe product fraction was evaporated

الإجراء التجريبي

A mixture of 1.5 g (5.6 mmoles) 2-amino-6-chloro-4-n-pentyloxypteridine (e.g. available following the procedure disclosed by Mohr et al. in Helv. Chem. Acta (1992) 75:2317), palladium acetate (63 mg, 0.28 mmoles), tri-o-tolylphosphane (682 mg, 2.24 mmoles), cuprous iodide (53 mg, 0.28 mmoles), styrene (1,3 ml., 11.3 mmoles) and triethylamine 3.1 ml, 22 mmoles) was stirred in dry acetonitrile (50 ml) under reflux for 90 hours. It was evaporated and the residue purified by silica gel column chromatography with chloroform. The product fraction was evaporated to give 1.37 g (yield: 72%) of an orange powder exhibiting, after recrystallization from a EtOAc/hexane mixture, a melting point (m.p.) range of 127–128° C.

المصدر