HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl azodicarboxylate → HCID 135830955, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | HCID 22144502 | HCID 22144502 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 135830955 | HCID 135830955 | 92.4% |
Reaction Steps
2-Chloro-N-(2-chloro-6-hydroxy-4-methoxy-phenyl)-4-methoxy-benzamide (40 mg) was completely dissolved in THF (5 mL) and PPH3 (46 mg) was added and the mixture was stirred until all PPH3 dissolved. To this mixture was added drop wise DEAD (0.03 mL) diluted in THF (0.5 mL). The mixture was stirred at room temperature for 2 h and the reaction mixture was diluted with ethyl acetate and washed with water, brine, dried over MgSO4 and concentrated. Flash chromatography on silica gel eluting with 10% to 30% ethyl acetate-hexane afforded 32 mg (85%) of the title compound as a solid. MS: 324 (MH+), HPLC tR: 3.18 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07045539B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-26e1231cb28d41598882a5362e736e5f |
| Source note | uspto-grants-2006_05 |