HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine → 5-Bromo-2-(dimethylamino-methyleneamino)-3-methyl-benzoic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine | HCID 547712 | — |
| Reactant | 2-Amino-5-bromo-3-methylbenzoic acid | HCID 11850383 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-Bromo-2-(dimethylamino-methyleneamino)-3-methyl-benzoic acid tert-butyl ester | HCID 54014692 | 97.5% |
Reaction Steps
A mixture of 5.0 g (21.7 mmol) of the product of Example 132 and 20.8 ml (86.9 mmol) of N,N-dimethylformamide di-t-butylacetal in 30 ml of toluene was heated to reflux for 2 hr. The reaction mixture was cooled to room tenperature, washed with water and brine, dried over MgSO4 and concentrated in vacuo to provide 3.61 g (49%) of the desired product as an yellow oil. Electrospray Mass Spec 341(M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05929097 |
| Source dataset | uspto-grants-1999_07 |
| ORD ID | ord-fb49ab09e1cc4f558dd63dc41eccd7fe |
| Source note | uspto-grants-1999_07 |