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2-Benzofurancarbonyl chloride → HCID 68710769、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Benzofurancarbonyl chloride | HCID 38949 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | methyl N-[(4'-amino-1,1'-biphenyl-4-yl)sulfonyl]-N-methyl-D-valinate | HCID 59150916 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 68710769 | HCID 68710769 | 86.6% |
反応手順
To 0.11 g of methyl N-[(4′-amino-1,1′-biphenyl-4-yl)sulfonyl]-N-methyl-D-valinate in 4 mL dichloromethane cooled in ice bath, was added 0.058 g of 2-benzofurancarbonyl chloride, and N,N-diisopropylethylamine (0.15 mL) was dropped in. The reaction was stirred at room temperature overnightand then diluted with dichloromethane. The organic layer was washed with water, 5% HCl, and brine, dried over sodium sulfate, filtered, concentrated, and purified by column chromatography eluting with hexane:ethyl acetate (2:1) to provide 0.13 g of methyl N-({4′-[(1-benzofuran-2-ylcarbonyl)amino]-1,1′-biphenyl-4-yl}sulfonyl)-N-methyl-D-valinate. Yield 86.6%. m.p. 67-69° C. MS: 521.3 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420001B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-0587f10292e2495193029e1e95053a0f |
| 出典メモ | uspto-grants-2008_09 |