HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 1h-Indole-1-carboxylic acid,5-[(dimethylamino)methyl]-,1,1-dimethylethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | Indole-5-carboxaldehyde | HCID 589040 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1h-Indole-1-carboxylic acid,5-[(dimethylamino)methyl]-,1,1-dimethylethyl ester | HCID 68491935 | 36.2% |
Reaction Steps
In a similar manner to Step 1 of Reference Example 4, 5-formylindole (5.27 g, 36.3 mmol) was dissolved in acetonitrile (100 mL), and the solution was treated with di-tert-butyldicarbonate (9.17 mL, 39.9 mmol) and DMAP (44.0 mg, 0.360 mmol), then the mixture was treated with 51% aqueous dimethylamine solution (72.0 mL, 724 mmol), acetic acid (41.6 mL, 727 mmol) and sodium triacetoxyborohydride (46.2 g, 218 mmol), followed by purification by slurry using diisopropyl ether to obtain 5-(dimethylaminomethyl)-1-(tert-butoxycarbonyl)indole (3.61 g, yield 36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07745641B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-59d0630de42b4180826f17821e743067 |
| Source note | uspto-grants-2010_06 |