HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 67083692, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Dithionite | HCID 24489 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 67083679 | HCID 67083679 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67083692 | HCID 67083692 | 115.6% |
Reaction Steps
A suspension of sodium dithionite (978 mg, 4.21 mmol) and 4-(2-fluoro-4-iodo-phenylamino)-5-nitro-indazole-1-carboxylic acid tert-butyl ester (700 mg, 1.4 mmol) in water (35 mL) was treated with a 1:1 mixture of THF:dioxane (34 mL), the homogeneous reaction mixture stirred at room temperature for 4 hours. Further sodium dithionite (978 mg, 4.21 mmol) was added and stirring continued for 20 hours. The reaction mixture was basified by the addition of saturated aqueous sodium hydrogen carbonate and then extracted with ethyl acetate (150 mL). The organic extract was washed with water, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a yellow solid (758 mg, quant.). LCMS (Method B) RT=4.09 min, [M+H]+=469.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841462B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-bdf00e9c514b48ef86e3aa29408ecc2c |
| Source note | uspto-grants-2014_09 |