HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 22013032, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Bromo-1,1-dimethoxyethane | HCID 81672 | — |
| Reactant | 3,3-Dimethoxy-1,3-dihydro-2H-indol-2-one | HCID 15480745 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22013032 | HCID 22013032 | 50.3% |
Reaction Steps
A solution of 34.3 g of 3,3-dimethoxyindolin-2-one in 400 ml of N,N-dimethylformamide was added dropwise to a suspension of 8.56 g of sodium hydride (60%) in 100 ml of N,N-dimethylformamide at 0° C. in a nitrogen stream. After the mixture was stirred at that temperature for 30 minutes, 36.2 g of bromoacetaldehyde dimethyl acetal was added thereto. The resulting mixture was stirred at 80° C. for 1 day and then concentrated. Ethyl acetate was added to the residue, and the mixture was washed with an aqueous solution of sodium chloride. The organic layer was dried over anhydrous sodium sulfate and concentrated. The resulting crude product was recrystallized from isopropyl alcohol/hexane to give 25.1 g (50%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06031111 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-b72edb3b143b4b7d96d0aa2452c52a94 |
| Source note | uspto-grants-2000_02 |