HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N,N',N'-Tetramethylmethanediamine → 4-NITROGRAMINE
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N,N',N'-Tetramethylmethanediamine | HCID 5829 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-Nitro-1H-indole | HCID 145766 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 4-NITROGRAMINE | HCID 251453 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
N,N,N′,N′-Tetramethyldiaminomethane (2.2 mL, 15.6 mol) in acetic acid (30 mL) was added dropwise over 60 min to a solution of 4-nitroindole (2.30 g, 14.2 mol) in acetic acid (30 mL). After 3.5 h, the reaction was cooled to 0° C., and 20% aqueous sodium hydroxide was added to adjust the pH to 11. The mixture was extracted with CHCl3 (3×300 mL) and the combined organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo to give the title compound. MS: m/z=220 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696192B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-c97b48404fac44f9840ac7f7e9cc1dca |
| Source note | uspto-grants-2010_04 |