반응 #62612

반응 방정식

oxalyl chloride

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

→

brown crystalline solid

수율 82.3%

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

수율 82.3%

용매

diethyl ether

ether

반응 조건

후처리

1. 1
   기타prepared
2. 2
   기타was removed under reduced pressure
3. 3
   기타The residue was triturated with isopropyl ether/hexane

실험 절차

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).

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