HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 10343819, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 67156830 | HCID 67156830 | — |
| Reactant | HCID 131728846 | HCID 131728846 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10343819 | HCID 10343819 | — |
Reaction Steps
Oxone (0.52 g, 0.84 mmol) in water (4 mL), buffered to pH ˜6 with sodium oxide acetate, was added to 2-[(4-tert-butylphenyl)thio]-4-piperazin-1-ylthieno[3,2-c]pyridine (0.42 mmol) in ethanol (30 mL). The mixture was stirred in room temperature for 2 h and more oxone (0.52 g, 0.84 mmol) was added. The reaction was stirred over night. Water was added to the mixture, extraction with dichloromethane (2×20 mL) and the solvent was removed. The products were purified by preparative HPLC. Yield: 41.9 mg (22.0%). 1H NMR (500 MHz, CH3OH-d4) δ ppm 8.38 (s, 1H) 8.05-8.01 (m, 3H) 7.80 (d, J=6.59 Hz, 1H) 7.71-7.69 (m, 2H) 4.15-4.13 (m, 4H) 3.59-3.57 (4H) 1.37-1.33 (m, 9H); LC-MS 416 (M−H)+; Purity (HPLC) 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07943639B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-fab7cdb9da4d4a2da52e7aff0a8ea638 |
| Source note | uspto-grants-2011_05 |