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Tetrahydrofuran → 4-methoxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | 4-hydroxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one | HCID 76168310 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-methoxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one | HCID 74020005 | — |
反応手順
To a mixture of 5 ml of tetrahydrofuran and 6 ml of dichloromethane were added 0.59 g of 4-hydroxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one, 0.45 g of triphenylphosphine and 55 mg of methanol, and to the mixture was added dropwise 0.74 g of a 40% toluene solution of diethyl azodicarboxylate. The mixture was stirred at room temperature for 40 minutes, and the reaction mixture was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.18 g of 4-methoxy-3-[3-[3-(methoxyacetylamino)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one [Compound No. (22d)].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07691883B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-c3ef72fda628464293ddb6a778e9f6bb |
| 出典メモ | uspto-grants-2010_04 |