HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 86701006, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | HCID 26596852 | HCID 26596852 | — |
| Reactant | (2S,5R)-6-(Benzyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carboxylic acid | HCID 57389355 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86701006 | HCID 86701006 | 54% |
Reaction Steps
DIPEA (3.7 g, 10 mmol) was added to a solution of (2S,5R)-6-(benzyloxy)-7-oxo-1,6-diaza-bicyclo[3.2.1]octane-2-carboxylic acid (1.45 g, 5.3 mmol) and tert-butyl 4-(hydrazinecarbonyl)piperazine-1-carboxylate, (1.6 g, 6.6 mmol) in dry DMF (50 mL) at 0° C., followed by the addition of HATU (1.45 g, 5.3 mmol). The reaction mixture was stirred at rt overnight. The mixture was diluted with water (200 mL), and the resulting precipitation was collected by filtration, rinsed with water, and then recrystallized (3:1 petroleum ether/EtOAc) to afford tert-butyl 4-(2-((2S,5R)-6-(benzyloxy)-7-oxo-1,6-diazabicyclo[3.2.1]octane-2-carbonyl)hydrazinecarbonyl)piperazine-1-carboxylate (1.4 g, 54%), ESI-MS (EI+, m/z): 503 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969570B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-03516c46b34541e99ddb44fd211d3805 |
| Source note | uspto-grants-2015_03 |