関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Fluoro-4-nitrobenzyl alcohol | HCID 2774658 | — |
| 反応物 | HCID 178457872 | HCID 178457872 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178457837 | HCID 178457837 | 71.5% |
反応手順
To a suspension of cis-4-amino-N-isopropylcyclohexanecarboxamide hydrochloride (7.09 g, 32.1 mmol) and DIPEA (15 mL, 88 mmol) in ACN (50 mL) was added (3-fluoro-4-nitrophenyl)methanol (5 g, 29.2 mmol). The reaction was stirred overnight at 80° C. The reaction mixture was concentrated, loaded onto a silica-gel pre column, and purified by column chromatography, eluting with 0-100% EtOAc in DCM, to provide cis-4-(5-(hydroxymethyl)-2-nitrophenylamino)-N-isopropylcyclohexanecarboxamide as an orange foam (7.0 g, 71.4% yield). MS, m/z (C17H25N3O4): calcd, 335.2. found, 336.0 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09115127B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
|---|
| ORD ID | ord-93c854b547344db3a1358d1d90e9b33b |
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| 出典メモ | uspto-grants-2015_08 |
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