تفاعل #62612

معادلة التفاعل

oxalyl chloride

4-[trimethyl[silyl]oxy]-2H-benzothiopyran

→

brown crystalline solid

المردود 82.3%

4H-[1]-Benzothiopyrano[4,3-b]furan-2,3-dione

المردود 82.3%

المذيبات

diethyl ether

ether

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared
2. 2
   أخرىwas removed under reduced pressure
3. 3
   أخرىThe residue was triturated with isopropyl ether/hexane

الإجراء التجريبي

To a stirred mixture of 4-[trimethyl[silyl]oxy]-2H-benzothiopyran (380.5 g, 1.609 mol), prepared according to the method of L. Hellberg et al, Tet. Letters, 3553-3554 (1974), and one liter of diethyl ether, were added 103.8 g (0.818 mol) of oxalyl chloride in a dropwise manner over a period of 50 minutes at room temperature under nitrogen. The mixture was stirred at room temperature for 17 hours after which time the ether was removed under reduced pressure. The residue was triturated with isopropyl ether/hexane to give 146.9 g (82.3%) of a brown crystalline solid, mp 156° C. (dec).

المصدر