反応 #74293

反応方程式

DMRIE

chloroform

→

CHCl3 MeOH NH4OH H2O

反応条件

後処理

1. 1
   洗浄washed with 3 mL 1N HCl
2. 2
   乾燥The organic phase was dried with MgSO4
3. 3
   ろ過filtered into a reaction vessel
4. 4
   その他The solution was placed in an ice-water bath
5. 5
   workup.ADDITIONN-hydrosuccinimide (82 mg) then dicyclohexylcarbodiimide (1.3 mL of a 0.5 M solution in dichloromethane) were added
6. 6
   温度with warming for 8 hours
7. 7
   workup.ADDITIONAt this time propyl amine (40 mg) was added as a neat liquid
8. 8
   workup.STIRRINGto stir at room temperature overnight
9. 9
   ろ過The reaction was filtered
10. 10
    その他evaporated

実験手順

DMRIE-Ox (300 mg) was dissolved in 7 mL chloroform and washed with 3 mL 1N HCl. The organic phase was dried with MgSO4, then filtered into a reaction vessel. The solution was placed in an ice-water bath and N-hydrosuccinimide (82 mg) then dicyclohexylcarbodiimide (1.3 mL of a 0.5 M solution in dichloromethane) were added and the reaction was allowed to stir with warming for 8 hours. At this time propyl amine (40 mg) was added as a neat liquid and the reaction allowed to stir at room temperature overnight. The reaction was filtered, then evaporated. Chromatography of the filtrate residue through silica gel with CHCl3:MeOH:NH4OH:H2O (90:10:0.25:0.25) afforded pure product.

出典