HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 135830952, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | HCID 135830956 | HCID 135830956 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 135830952 | HCID 135830952 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To 2-(2-chloro-4-hydroxy-phenyl)-7-iodo-benzooxazol-5-ol (279 mg) in DMF (5 mL) was added CuCN (97 mg). The mixture was placed in an oil bath and heated to 150° C. for 3 h. The mixture was cooled to room temperature and diluted with ethyl acetate and washed with 1N HCl, saturated aqueous EDTA, brine (3×), dried (Na2SO4), and concentrated. Material was purified by preparative LC/MS. MS: 278 (MH+), HPLC tR: 1.92 min. The HPLC conditions used are the following: HPLC Waters Corp. Novapak HR™ C 18 RCM 40×100 mm 6 μm particle; flow rate 40 mL/min, linear gradient from 35% B to 65% B over 15 min; A=water, 0.1% TFA; B=MeOH, UV detection at 254 nm and positive ionization mass spectrometry detection
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07045539B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-6cd4f5521fab416c9cbe0eb2edb80d22 |
| Source note | uspto-grants-2006_05 |