反応 #320977

反応方程式

(4R)-4-(di-n-propylamino)-1,3,4,5-tetrahydrobenz[cd]indole-6-carboxylic hydrazide

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title compound

収率 163.9%

(-)(4R)-6-(5-phenyl-1,3,4-oxadiazol-2-yl)-4-(di-n-propylamino)-1,3,4,5-tetrahydrobenz[cd]indole

収率 163.9%

溶媒

trimethylorthobenzoate

methylene chloride

反応条件

後処理

1. 1
   温度After cooling
2. 2
   抽出the product was extracted into aqueous tartaric acid
3. 3
   抽出the product was extracted into methylene chloride
4. 4
   その他Evaporation of the methylene chloride
5. 5
   workup.WAITleft crystalline product which
6. 6
   その他was then chromatographed over 3 g of silica gel
7. 7
   その他The product from the column was recrystallized from toluene

実験手順

A solution of 0.20 g (0.64 mmol) of (4R)-4-(di-n-propylamino)-1,3,4,5-tetrahydrobenz[cd]indole-6-carboxylic hydrazide in 2.0 ml of trimethylorthobenzoate was heated at 135° C. under nitrogen for 5 hours. After cooling, the semisolid mixture was dissolved in methylene chloride and the product was extracted into aqueous tartaric acid. The aqueous solution was basified with sodium carbonate and the product was extracted into methylene chloride. Evaporation of the methylene chloride left crystalline product which was then chromatographed over 3 g of silica gel using ethyl acetate as eluent. The product from the column was recrystallized from toluene to give 0.21 g of title compound.

出典