関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-[(1,1-Dimethylethoxy)carbonyl]-L-leucine 4-nitrophenyl ester | HCID 1810201 | — |
| 反応物 | H-Ser-Thr-OBzl.TFA | HCID 131711572 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | BOC-Leu-Ser-Thr-OBzl | HCID 131711574 | — |
反応手順
52.5 g of H-Ser-Thr-OBzl.TFA are dissolved in 145 ml of dimethylformamide and mixed at 0° C. with a solution of 48.0 g of BOC-Leu-ONP. 21 ml of triethylamine and 0.75 ml of glacial acetic acid are then added. The reaction mixture is stirred for 3 hours at 0° C. and overnight at room temperature. After adding 2.1 liters of ethyl acetate the solution is extracted by shaking twice with water, twice with 0.1 N hydrochloric acid, twice with 10% strength sodium chloride solution, eight times with 20% strength potassium carbonate solution, twice with 10% strength sodium chloride solution and once with 30% strength sodium chloride solution. After drying over sodium sulphate the solution is concentrated to about 1.4 liters. The protected tripeptide of melting point 114°-116° C. crystallises overnight in the refrigerator; [α]D -14° (c = 2 in dimethylformamide); Rf2 = 0.25 (on silica gel).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04159981 |
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| 出典データセット | uspto-grants-1979_07 |
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| ORD ID | ord-cf4850c7610342bca7e023d4ebac8c36 |
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| 出典メモ | uspto-grants-1979_07 |
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