Reaktion #591618

Reaktionsgleichung

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe volatiles were removed in-vacuo
2. 2
   Sonstigethe residue was purified by CombiFlash
3. 3
   Wascheneluting with 0 to 30% EtOAc in hexane
4. 4
   Sonstigeto provide the THF compound

Vorschrift

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.

Quelle