Реакция #591618

Уравнение реакции

tert-butyl 3-iodo-4,4-dimethyl-1-oxa-7-azaspiro[4.4]nonane-7-carboxylate

tris(trimethylsilyl)silane

2,2′-azo-bis-isobutyronitrile

toluene

→

tert-butyl 4,4-dimethyl-1-oxa-7-azaspiro[4.4]nonane-7-carboxylate

Условия реакции

Обработка

1. 1
   ДругоеThe volatiles were removed in-vacuo
2. 2
   Другоеthe residue was purified by CombiFlash
3. 3
   Промывкаeluting with 0 to 30% EtOAc in hexane
4. 4
   Другоеto provide the THF compound

Методика

A mixture of tert-butyl 3-iodo-4,4-dimethyl-1-oxa-7-azaspiro[4.4]nonane-7-carboxylate (0.47 g, 0.0012 mol), tris(trimethylsilyl)silane (0.456 mL, 0.00148 mol) and 2,2′-azo-bis-isobutyronitrile (0.002 g, 0.00001 mol) in toluene (10.00 mL, 0.09388 mol) was heated at 90° C. overnight. The volatiles were removed in-vacuo and the residue was purified by CombiFlash, eluting with 0 to 30% EtOAc in hexane, to provide the THF compound. LCMS (M+Na) 278.2.

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