HuagongsheHuagongshe Chemistry Print Report · For research reference only
(3-Methoxy-1-propynyl)tributylstannane → 2-(3-Methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (3-Methoxy-1-propynyl)tributylstannane | HCID 10872067 | — |
| Reactant | 2-Chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester | HCID 86664331 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2-(3-Methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester | HCID 86664332 | 63.1% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 700 mg (2.6 mmol) 2-chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester and 1.39 g (3.9 mmol) tributyl(3-methoxyprop-1-ynyl)stannane in dioxane (10 ml) was added 273 mg (0.39 mmol) PdCl2(PPh3)2. Then the reaction solution was heated at 100° C. for 16 h. After cooling to RT the mixture was filtered through celite and the filtrate was concentrated in vacuo. The residue was dissolved in EtOAc and washed with water. The organic layer was dried over Na2SO4 and concentrated in vacuo. Purification of the residue by CC (5% KF-silica, hexane/EtOAc 19:1) provided 500 mg (1.64 mmol, 63%) 2-(3-methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09168259B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-3fd6e8ee9f25422db59d7bad1cd01900 |
| Source note | uspto-grants-2015_10 |