関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | Lysine hydrochloride, D- | HCID 81691 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | D-2-Aminohexano-6-lactam | HCID 439823 | — |
反応手順
To a solution of (R)-lysine HCl salt (100 g, 0.68 mol) in xylene (1 L) was added hexamethyldisilazane (1000 mL, 4.76 mol) and chlorotrimethylsilane (10 mL, 78.8 mmol). The mixture was heated to 120° C. for 24 h, then to 180° C. for 48 h. The solvent was then removed under reduced pressure and the crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH) to afford (R)-3-aminoazepan-2-one (I-1a).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440957B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-6d4b5949406f44f498638a066d6521b7 |
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| 出典メモ | uspto-grants-2016_09 |
|---|
