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Triethylamine → N-[(4'-nitro-1,1'-biphenyl-4-yl)sulfonyl]-D-valine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | D-Valine | HCID 71563 | — |
| 反応物 | 4'-Nitrobiphenyl-4-sulfonyl chloride | HCID 2760185 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-[(4'-nitro-1,1'-biphenyl-4-yl)sulfonyl]-D-valine | HCID 68708071 | 92.6% |
反応手順
To 0.117 g of D-valine in 2.5 mL dioxane and 2.5 mL of water, cooled in an ice bath, was added 0.31 g of 4′-nitro-1,1′-biphenyl-4-sulfonyl chloride, followed by 0.4 mL of triethylamine, The reaction was then stirred at room temperature overnight. After concentrating the reaction mixture in vacuo, the residue was extracted with ethyl acetate and 1N HCl. The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo to provide 0.35 g of N-[(4′-nitro-1,1′-biphenyl-4-yl)sulfonyl]-D-valine as a solid. Yield 74.5%. m.p. 165-167° C.; MS: 377.0 (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-4b1a9f1f172a4d3c90c461b5ee9970d7 |
| 出典メモ | uspto-grants-2008_09 |