HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butoxy bis(dimethylamino)methane → HCID 89631940, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butoxy bis(dimethylamino)methane | HCID 79885 | — |
| Reactant | HCID 89618125 | HCID 89618125 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 89631940 | HCID 89631940 | 97% |
Reaction Steps
A solution of the tert-butyl 5-allyl-2-oxo-3,3a,4,8b-tetrahydroindeno[1,2-b]pyrrole-1-carboxylate (Step 4, 0.21 g, 0.7 mmol) in tert-butoxybis(dimethylamino)methane (0.415 mL, 2.0 mmol) in toluene (3 ml) was heated at 110° C. overnight. The solution was diluted with ethyl acetate and washed twice with water, brine, dried over magnesium sulphate and concentrated to give tert-butyl (3Z)-5-allyl-3-(dimethylaminomethylene)-2-oxo-4,8b-dihydro-3aH-indeno[1,2-b]pyrrole-1-carboxylate D1 (colourless solid, 0.24 g, 97%). This compound was used without extra purification. LC-MS (Method C) RT 1.05 min, 369 (M+H+). This method was used to prepare compound D2 to D13 (table D).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09210929B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-a6989bd35f4d469bb4f375273453173f |
| Source note | uspto-grants-2015_12 |