HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-methylacetoacetate → HCID 15716741, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-methylacetoacetate | HCID 701 | — |
| Reactant | Benzylamine | HCID 7504 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 15716741 | HCID 15716741 | 104.8% |
Reaction Steps
A solution of ethyl 2-methylacetoaceate (1-004-01) (115.34 g) and benzylamine (85.73 g) in toluene (1.6 L) was azeotropically dehydrated in an oil bath at 145° C. for 8 h under nitrogen atmosphere. Benzylamine was added to the reaction mixture and the reaction mixture was dehydrated again. After 6 h, the reaction mixture was distilled under atmospheric pressure to remove about 600 mL of the solvent, and evaporated under reduced pressure to give ethyl 3-benzylamino-2-methylcrotonate (1-004-02) (195.66 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06977266B2 |
| Source dataset | uspto-grants-2005_12 |
| ORD ID | ord-4dbe1bbe51954820baaac630430ea38e |
| Source note | uspto-grants-2005_12 |