HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-Dimethylaminomethyl-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | N,N-dimethylmethyleneammoniumiodide | HCID 21892197 | — |
| Reactant | 4-Hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester | HCID 66713092 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Dimethylaminomethyl-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester | HCID 66713173 | 16.6% |
Reaction Steps
A mixture of 4-Hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester (177 mg, 0.5 mmol; see example D-1f), N,N-dimethylmethyleneammonium iodide (94 mg, 0.5 mmol), K2CO3 (104 mg, 0.75 mmol), and anhydrous CH2Cl2 (3 ml) was stirred at ambient temperature for 2.5 d before the mixture was concentrated in vacuo. To the residue was added water (15 ml), the mixture was acidified by addition of 6 N HCl and then washed with Et2O (3×30 ml). Subsequently, the mixture was neutralized by the addition of concentrated aqueous NaHCO3 and extracted with EtOAc (20 ml). The organic phase was dried over MgSO4 and concentrated in vacuo to give the title compound as a dark oil (34 mg); MS-(+)-ion M+1=411.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916585B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-e66483b85c084f01ad99c60b6481f77d |
| Source note | uspto-grants-2014_12 |