HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 58465597, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 5-(Pyridin-2-yl)thiophene-2-carboxylic acid | HCID 736482 | — |
| 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 58465821 | HCID 58465821 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58465597 | HCID 58465597 | — |
Reaction Steps
To a mixture of ethyl 5,6,7,8-tetrahydro-4H-pyrazolo[1,5-a][1,4]diazepine-2-carboxylate (0.033 g, 0.16 mmol) and 5-(2-pyridyl)thiophene-2-carboxylic acid (0.036 g, 0.18 mmol) in methylene chloride (1 mL) was added N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (0.07 g, 0.184 mmol) and N-methylmorpholine (0.053 mL, 0.48 mmol). The reaction was stirred overnight at room temperature. The reaction was diluted with methylene chloride (3 mL) and washed with saturated aqueous NaHCO3 (2 mL). The aqueous layer was extracted with additional methylene chloride (3 mL). The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated to dryness to afford Intermediate 31.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946223B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-ce79fd6a70d04a61afaa73b82fefe903 |
| Source note | uspto-grants-2015_02 |