HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 117902800, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | HCID 117902632 | HCID 117902632 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 117902800 | HCID 117902800 | — |
Reaction Steps
A crude reaction mixture from the preparation of 1-(2,6-diazidopyridin-4-yl)-7-methyl-1H-indole G1 (approx. 340 mg, 1.2 mmol in 2 ml crude mixture) is diluted with EtOAc (10 ml). Under an atmosphere of nitrogen palladium on activated charcoal (10 mg, 10% Pd) is added. At RT the atmosphere is replaced by hydrogen (5 bar) and stirring is continued for 24 h. The mixture is filtered and extracted with an aqueous 0.5 mol/l sodium hydroxide solution. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by RP HPLC. Yield: 120 mg (43%). HPLC-MS: M+H=239; tR=0.81 min (Method—2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249151B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-ac01ed4bff0f4f59a1560747c985addf |
| Source note | uspto-grants-2016_02 |