反応 #62612

反応方程式

oxalyl chloride

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

→

brown crystalline solid

収率 82.3%

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

収率 82.3%

溶媒

diethyl ether

ether

反応条件

後処理

1. 1
   その他prepared
2. 2
   その他was removed under reduced pressure
3. 3
   その他The residue was triturated with isopropyl ether/hexane

実験手順

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).

出典