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2-Diazonio-1-ethoxyprop-1-en-1-olate → HCID 178438752、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Diazonio-1-ethoxyprop-1-en-1-olate | HCID 53440922 | — |
| 反応物 | HCID 178438743 | HCID 178438743 | — |
| 触媒 | Acetic acid, rhodium(2+) salt | HCID 21674 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178438752 | HCID 178438752 | — |
反応手順
To a mixture of 3′-fluoro-4′-{[4-(cis-3-hydroxycyclobutyl)-2-methyl-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (659 mg), rhodium(II) acetate (dimer) (31 mg) and methylene chloride (5 mL) was added dropwise ethyl 2-diazopropanoate (359 mg) under an argon atmosphere at 70° C., and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by basic silica gel chromatography [eluent: hexane/ethyl acetate=90/10→70/30 (volume ratio)] to give the title compound as a colorless amorphous compound (553 mg, 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115136B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-efe32d49970d46bda5b4b1777fec99dd |
| 出典メモ | uspto-grants-2015_08 |