HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67299188, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | HCID 67187947 | HCID 67187947 | — |
| Reactant | HCID 67299299 | HCID 67299299 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 67299188 | HCID 67299188 | 119.1% |
Reaction Steps
0.3 g of the compound obtained in stage 22A), 0.3 g of 4,4-difluoro-1,4′-bipiperidine-4′-carboxamide (described in Preparation 5, page 23, of Application WO 2008/068423), 0.45 ml of Et3N and 0.25 g of TBTU are added in order to 10 ml of CH2Cl2. After 3 hours at AT, the mixture is concentrated to dryness and the residue is taken up in AcOEt, washed with water, dried and concentrated to dryness. After purifying by chromatography on silica (elution gradient: CH2Cl2 up to CH2Cl2/MeOH 98/2), the compound obtained is dissolved in CH2Cl2, ethereal hydrochloric acid is added down to a pH of 1 and then the mixture is concentrated to dryness. 0.28 g of the expected compound is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410137B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-f0ff4dd273954e44a47b04864aea8984 |
| Source note | uspto-grants-2013_04 |