HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-butyl 1-[[(2S)-1-[(Z)-1-aminoethylideneamino]oxy-3,3-dimethyl-1-oxobutan-2-yl]carbamoyl]-3-phenyl-6,8-dihydro-5H-imidazo[1,5-a]pyrazine-7-carboxylate → (S)-tert-butyl 1-(2,2-dimethyl-1-(3-methyl-1,2,4-oxadiazol-5-yl)propylcarbamoyl)-3-phenyl-5,6-dihydroimidazo[1,5-a]pyrazine-7(8H)-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-butyl 1-[[(2S)-1-[(Z)-1-aminoethylideneamino]oxy-3,3-dimethyl-1-oxobutan-2-yl]carbamoyl]-3-phenyl-6,8-dihydro-5H-imidazo[1,5-a]pyrazine-7-carboxylate | HCID 57635411 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Product | (S)-tert-butyl 1-(2,2-dimethyl-1-(3-methyl-1,2,4-oxadiazol-5-yl)propylcarbamoyl)-3-phenyl-5,6-dihydroimidazo[1,5-a]pyrazine-7(8H)-carboxylate | HCID 57635507 | 88.1% |
Reaction Steps
Intermediate 22C (0.20 g, 0.39 mmol) was dissolved in a 1N solution of TBAF in THF (0.55 mL). The resulting mixture was stirred overnight, concentrated, diluted with EtOAc and washed successively with water and brine, dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified by preparative flash chromatography on silica, eluting with a 20-70% ethyl acetate/hexanes gradient to provide Intermediate 22D (0.17 g, 88%). 1H-NMR (400 MHz, CDCl3-d) δ: 1.09 (s, 9H), 1.51 (s, 9H), 2.40 (s, 3H), 3.78 (m, 2H), 4.11 (m, 2H), 5.01 (m, 2H), 5.37 (d, 1H), 7.35 (m, 3H), 7.64 (m, 2H), 7.78 (d, 1H); LCMS (+ESI) m/z 495.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859538B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-e18927ec7ab54234bc1121562f6a6712 |
| Source note | uspto-grants-2014_10 |