HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 90060615, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Reactant | (2S)-2-(((tert-butoxy)carbonyl)(methyl)amino)propanoic acid | HCID 7009590 | — |
| Reactant | HCID 42614160 | HCID 42614160 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Product | HCID 90060615 | HCID 90060615 | 270% |
Reaction Steps
3-Amino-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride (1.0 g, 5.15 mmol, Eq: 1.00), BOC—N-Me-Ala-OH (1.26 g, 1.62 mmol, Eq: 1.2) and TEA (2.2 mL, 15.45 mmol, Eq: 3.00) were dissolved in DMF (30 mL) and HOBT.H2O (697 mg, 5.14 mmol, Eq: 1.20) and HBTU (2.34 g, 6.18 mmol, Eq: 1.20) were added. After 1 h 20 min. the mixture was diluted with 1 N HCl and extracted with EtOAc. The organic extracts were washed with 1 N NaOH, brine, dried over Na2SO4 and concentrated to afford the title compound (1.66 g, 85% yield) which was used without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394263B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-91e24da3a02f4f8195c7113847b5340a |
| Source note | uspto-grants-2016_07 |