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Lawesson's reagent → 1,1-Dimethylethyl N-[(1S)-1-(aminothioxomethyl)-2-methylpropyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | Boc-L-valine amide | HCID 11241393 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,1-Dimethylethyl N-[(1S)-1-(aminothioxomethyl)-2-methylpropyl]carbamate | HCID 11020776 | 70% |
反応手順
Boc-valineamide (0.5 g) was stirred in dry THF at room temperature under argon. Lawesson's reagent (1.56 g, 0.6 eq) was added and the mixture was stirred overnight. The solvent was evaporated and the residue chromatographed (silica, 2.5% methanol/dichloromethane) to give the title compound as a white solid (0.373 g, 70%). NMR(CDCl3) δ 8.59 (1H, br s), 8.09 (1H, br s), 5.41 (1H, d (br)), 4.20 (1H, dd), 1.99 (1H, m), 1.39 (9H, s), 0.90 (6H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733882 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-0a45a609ac2e45e08721ea94db9274b3 |
| 出典メモ | uspto-grants-1998_03 |