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(4-Nitrophenyl)acetic acid → di t-butyl 4-nitrobenzylcarbonyl-L-glutamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (4-Nitrophenyl)acetic acid | HCID 4661 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | L-Glutamic acid di-tert-butyl ester | HCID 208637 | — |
| 生成物 | di t-butyl 4-nitrobenzylcarbonyl-L-glutamate | HCID 86748613 | 77% |
反応手順
1-Hydroxybenzotriazole (4.05 g) was added to a solution of 4-nitrophenyl acetic acid (5.4 g) in dimethylformamide (75 ml). L-Glutamic acid di tert-butyl ester (7.77 g) and then dicyclohexylcarbodiimide (6.2 g) were added to the mixture. The mixture was then stirred for 18 hr at ambient temperature. The mixture was filtered and the filtrate washed with saturated sodium bicarbonate solution, water and 0.5 m hydrochloric acid and then dried and evaporated to dryness. The residue was chromatographed on silica gel by eluting with hexane/ethyl acetate (2:1) to give di t-butyl 4-nitrobenzylcarbonyl-L-glutamate as an oil 9.7 g (77%). NMR: 8.2(d)2H; 7.45(d)2H; 6.45(d)1H; 4.45(m)1H; 3.15(s)2H; 2.1(m)4H; 1.4(d)9H; 1.35(s)9H.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06277880B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-31560eb9abaa42709ee86dbe8a210f7f |
| 出典メモ | uspto-grants-2001_08 |