関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | N-(tert-butoxycarbonyl)glycine | HCID 78288 | — |
| 反応物 | p-Toluenesulfonate | HCID 85570 | — |
| 反応物 | Benzyl glycinate | HCID 409140 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Benzyl (tert-butoxycarbonyl)glycylglycinate | HCID 3244524 | 93.7% |
反応手順
Boc-Gly-OH (17.52 g, 0.1 mole) in a mixture of CHCl3 (50 ml) and acetonitrile (50 ml) was cooled to -15° C. and EDCI (19.17 g, 0.1 mole) was added and stirred for 20 minutes. To this, a pre-cooled solution of H-Gly-OBzl.tosylate (37.1 g, 0.11 mole), NMM (12.09 ml, 0.11 mole) in CHCl3 (100 ml) was added and stirred overnight at room temperature. After removing the solvent, the residue was taken in CHCl3 and extracted with acid and base. Chloroform was removed under reduced pressure, triturated with pet. obtain 30.2 g of I (yield: 93.7%), m.p. 82°-83° C. Rf2, 0.52; Rf4, 0.82. Anal. Cald. for C16H22N2O5 : C, 59.61; H, 6.88, N, 8.69%. Found: C, 59.43; H, 6.88; N, 8.35%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05064430 |
|---|
| 出典データセット | uspto-grants-1991_11 |
|---|
| ORD ID | ord-f8fa9cbcb0a64d688ab524bf26179d5f |
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| 出典メモ | uspto-grants-1991_11 |
|---|
