反応 #94209

反応方程式

hydrochloric acid

5-chloro-6-nitro-1-indanone

→

5-Chloro-6-amino-1-indanone

溶媒

ethanol

ethanol

反応条件

後処理

1. 1
   ろ過The precipitate is filtered off with suction
2. 2
   その他the product is precipitated from the hot filtrate by the addition of water
3. 3
   ろ過suction-filtered
4. 4
   洗浄washed with water
5. 5
   乾燥the filtrate is dried with Na2SO4
6. 6
   濃縮is then concentrated to dryness
7. 7
   その他after which process a further amount of the product is obtained
8. 8
   その他melts at a temperature of from 198° to 200° C.
9. 9
   その他is in the range of from 203° to 205° C.

実験手順

114 Grams (2.01 moles) of iron powder are added to a solution of 134 g (0.64 mole) of 5-chloro-6-nitro-1-indanone in 1600 ml of ethanol, then 63.5 ml of concentrated hydrochloric acid are added dropwise, and the reaction mixture is boiled for 4 hours. The precipitate is filtered off with suction, and the product is precipitated from the hot filtrate by the addition of water, then suction-filtered and washed with water. The residue of the reaction mixture is boiled with chloroform, the filtrate is dried with Na2SO4 and is then concentrated to dryness, after which process a further amount of the product is obtained. The substance melts at a temperature of from 198° to 200° C., and after recyrstallization from ethanol the melting point is in the range of from 203° to 205° C.

出典