HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 60141901, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 68295643 | HCID 68295643 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60141901 | HCID 60141901 | — |
Reaction Steps
To 100 mg (0.31 mmol) 2-Methoxy-5-(4-methyl-6-morpholin-4-yl-pyrimidin-5-ylethynyl)-pyridin-3-ylamine (E-9) in 5 mL DCM is added 70 mg (0.61 mmol) methanesulfonyl chloride and 72 μL (0.91 mmol) pyridine and the reaction mixture is stirred over night at RT. Water (2 mL) is added and the reaction mixture is extracted three times with 4 mL ethylacetate. The combined organic phases are dried over MgSO4 and concentrated under reduced pressure. The crude product is purified by RP chromatography (C18, 20-80% ACN in water containing 1% formic acid). Yield: 32 mg (18%). HPLC-MS: M+H=404; tR=0.65 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598157B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-b82accd0e1fa48f9ba044bf2eafc1044 |
| Source note | uspto-grants-2013_12 |