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Dichloromethane → Ammonia dichloromethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Diethylethanolamine | HCID 7497 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Di-tert-butyl diazene-1,2-dicarboxylate | HCID 6034084 | — |
| 反応物 | 4-Piperidin-1-ylmethyl-phenol | HCID 11636972 | — |
| 生成物 | Diethyl-[2-(4-piperidin-1-ylmethyl-phenoxy)-ethyl]-amine | HCID 11808427 | — |
| 生成物 | Ammonia dichloromethane | HCID 22731429 | 3% |
反応手順
A suspension of the product of Example 17 (176 mg), 2-Diethylamino-ethanol (0.12 mL), and polymer supported triphenylphosphine (613 mg; loading: 3 mmol/g) in DCM (5 mL) was treated with di-tert-butylazodicarboxylate (316 mg). After 2 h, the resulting mixture was filtered, and the filtrate was evaporated. Chromatography of the residue (3% 2 M methanolic ammonia/DCM) gave the title compound as a pale yellow oil (37 mg). 1H NMR (400 MHz, CDCl3): 7.20 (d, J=8.8 Hz, 2H), 6.84 (d, J=8.6 Hz, 2H), 4.03 (t, J=6.5 Hz, 2H), 3.40 (s, 2H), 2.87 (t, J=6.5 Hz, 2H), 2.63 (q, J=7.0 Hz, 4H), 2.35 (br s, 4H), 1.59-1.52 (m, 4H), 1.46-1.37 (m, 2H), 1.07 (t, J=7.1 Hz, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429586B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-9009b5b4fb8d4ce49b26ebb66249c190 |
| 出典メモ | uspto-grants-2008_09 |