HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57771773, compound → HCID 57771696, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57771773 | HCID 57771773 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | Ammonia | HCID 222 | 10% |
| Product | HCID 57771696 | HCID 57771696 | 195.9% |
Reaction Steps
Place methyl-(1-methyl-piperidin-3-yl)-(5-nitro-benzooxazol-2-yl)-amine (440 mg, 1.51 mmol) and iron powder (423 mg, 7.58 mmol) in acetic acid (10 mL). Heat the reaction to 40° C. for 2 h. Cool to rt and then load onto a Varian™ SCX column. Wash the column with methanol and DCM. Flush the compound off the column by eluting with 2M NH3 in methanol. Collect filtrate and concentrate in vacuo. Chromatograph (silica gel, eluting with 0-10% 2M NH3 in MeOH:DCM, then 10% 2M NH3 in MeOH:DCM) to yield 385 mg (98%) of the title compound: mass spectrum (ion-spray): (m/z)=261.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07838543B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-edc41679ed2346ec92d5590652fdfe01 |
| Source note | uspto-grants-2010_11 |