反応 #71575

反応方程式

3-{4-[(2-butyl-5-nitro-1-benzofuran-3-yl) carbonyl]phenoxy}propan-1-ol

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product

収率 91.0%

3-{4-[(5-amino-2-butyl-1-benzofuran-3-yl)carbonyl]phenoxy}propan-1-ol

収率 91.0%

溶媒

methanol

反応条件

後処理

1. 1
   workup.WAITThe mixture is left
2. 2
   温度maintaining the temperature below 40° C
3. 3
   その他Once the consumption of hydrogen
4. 4
   workup.WAITthe reaction is left
5. 5
   workup.STIRRINGunder stirring for approximately one further hour until it
6. 6
   その他reaches 25° C
7. 7
   ろ過The catalyst is filtered on a Celite panel
8. 8
   workup.ADDITIONthe alcoholic solution containing the product
9. 9
   濃縮is concentrated to residue
10. 10
    その他The crude product is crystallised
11. 11
    その他recovering it with 400 ml of toluene
12. 12
    その他the product is dried under a vacuum at 40° C. for 6-7 hours

実験手順

180 g (0.453 mol) of 3-{4-[(2-butyl-5-nitro-1-benzofuran-3-yl) carbonyl]phenoxy}propan-1-ol (formula(II)) dissolved in 1800 ml of methanol are loaded in a glass Buchi autoclave. Subsequently 9 g of Pd/C 10% (50% H2O) are added and H2 is loaded at a pressure of 4 bars. The mixture is left under stirring maintaining the temperature below 40° C. Once the consumption of hydrogen is complete, the reaction is left under stirring for approximately one further hour until it reaches 25° C. The catalyst is filtered on a Celite panel and the alcoholic solution containing the product is concentrated to residue. The crude product is crystallised, recovering it with 400 ml of toluene and the product is dried under a vacuum at 40° C. for 6-7 hours. 151 g of the product in the title are obtained.

出典