Reaktion #717774

Reaktionsgleichung

4-hydrazinyl-1-benzothiophene-7-carboxylic acid

methyl isopropyl ketone

→

2,3,3-trimethyl-3H-thieno[2,3-g]indole-5-carboxylic acid

Lösungsmittel

HOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeHOAc was removed in vacuo the product
2. 2
   Sonstigewas purified with CombiFlash silica gel column chromatography (eluted with CH2Cl2/MeOH stepping gradient 100:0 to 80:20)

Vorschrift

A solution of 4-hydrazinyl-1-benzothiophene-7-carboxylic acid CC (208 mg, 1.0 mmole) and methyl isopropyl ketone (457 mg, 5.3 mmole) in 5 mL HOAc was heated at 120° C. for 1.5 hr and cooled down to 25° C. HOAc was removed in vacuo the product was purified with CombiFlash silica gel column chromatography (eluted with CH2Cl2/MeOH stepping gradient 100:0 to 80:20). The yield of the desired product CD was 210 mg (81%).

Quelle