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Dimethylacetamide → HCID 178457235、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 3-Buten-1-amine | HCID 443732 | — |
| 反応物 | HCID 178486043 | HCID 178486043 | — |
| 生成物 | HCID 178457235 | HCID 178457235 | — |
反応手順
A solution of 420 mg (1.22 mmol) of trans-Methanesulfonic acid 3-[4-(tert-butoxycarbonyl-methyl-amino)-cyclohexyl]-prop-2-ynyl ester in 4 ml DMA was treated at 0° C. with 0.234 ml (2.43 mmol) of N-allylmethylamine and stirred at RT for 16 h. The solution was concentrated and the residual oil was extracted with aqueous sat. NaHCO3/Et2O (3×). The organic phases were washed with aqueous 10% NaCl solution and dried over Na2SO4 to yield after flash column chromatography on silica gel with hexane/EtOAc (2:1) 355 mg (91%) trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-carbamic acid tert-butyl ester, MS: 321 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858651B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-439d7e2d477a4a508227a0d6b50a1645 |
| 出典メモ | uspto-grants-2005_02 |