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Methane → HCID 178456073、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | (R)-1-Phenylpropylamine | HCID 5324978 | — |
| 反応物 | HCID 178482865 | HCID 178482865 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | HCID 178456073 | HCID 178456073 | 5.2% |
反応手順
A stirred solution of the product from Step 4 (2.00 g, 0.00711 mol), (R)-(+)-1-phenylpropylamine (1.06 g, 0.00784 mol), N-methylmorpholine (1.69 ml, 0.0154 mol) and isopropanol (13.3 ml) was refluxed, under nitrogen, until the reaction was shown to be complete by TLC (28 hours). It was then concentrated and the residue chromatographed on silica gel with 1 to 4% MeOH-CHCl3. A solution of the product thus obtained in MeOH-EtOAc was decolorized with Darco (activated charcoal) and crystallized from EtOAc-hexane to give 1.02 g, m.p. 109°-111° C. and 0.120 g, m.p. 107°-113° C. of the titled product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05567722 |
| 出典データセット | uspto-grants-1996_10 |
| ORD ID | ord-305b6d1802174bafaad6803f6180f433 |
| 出典メモ | uspto-grants-1996_10 |