反应详情

Warm mixture of 5-nitroindole (10 g, 62 mmol) and 200 mL glacial acetic acid to 70° C. and treat with Eschenmoser's salt (12 g, 65 mmol). Concentrate after 1 hour the reaction under vacuum to dryness. Mix the residue with 200 mL toluene, reconcentrate to dryness then partition between 200 mL concentrated ammonium hydroxide and 200 ml, EtOAc. When all solids dissolved, Separate the layers and extract the aqueous layer 200 mL EtOAc. Dry the combined organic layer over MgSO4 and concentrate to give N,N-dimethyl-5-nitrotryptamine as a solid.

1. temperatureWarm
2. concentrationConcentrate after 1 hour
3. customthe reaction under vacuum to dryness
4. customthen partition between 200 mL concentrated ammonium hydroxide and 200 ml, EtOAc
5. dissolutionWhen all solids dissolved
6. customSeparate the layers
7. extractionextract the aqueous layer 200 mL EtOAc
8. dry with materialDry the combined organic layer over MgSO4
9. concentrationconcentrate