HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86638389, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 130250-57-6 | HCID 14642623 | — |
| Reactant | 5-Oxo-(1,4)diazepane-1-carboxylic acid tert-butyl ester | HCID 22617736 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86638389 | HCID 86638389 | 98.7% |
Reaction Steps
To a cooled (0° C.) solution of 5-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester 5.9 g (28 mmol) and 4-bromo-N-methoxy-N-methyl-butyramide 5.4 g (28 mmol) in DMF (220 ml) was added NaH 1.3 g (30 mmol, 55% dispersion in oil), the mixture allowed to reach RT and the mixture stirred for a further 2 h. The reaction was then concentrated, the residue redissolved in EtOAc and washed with 10% aq. KHSO4 solution, brine, dried (MgSO4) and concentrated affording the title compound 9.1 g (quant) as white foam. MS: 330.3 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08138175B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-50f2f34f84034f4090c72a297f659ff2 |
| Source note | uspto-grants-2012_03 |