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Hydrochloric Acid → 2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-(2,3-Dihydro-1,4-benzodioxin-2-yl)acetonitrile | HCID 267531 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethanamine | HCID 55648 | — |
反応手順
The 2-cyanomethyl-(2,3 dihydrobenzo[1,4]dioxine) was dissolved in THF (50 mL) and 1M BH3 in THF (80 mL, 80 mmol) was added and the reaction mixture refluxed for 5 h, then stirred at ambient temperature for 16 h. With ice bath cooling, 2N HCl was added until pH=1.0 was achieved. The reaction mixture was then stirred for 1 h at room temperature and evaporated in vacuo to yield an oil. The oil was partitioned between 3N NaOH and diethyl ether, and the diethyl ether solution was washed with brine, dried (Na2SO4) and evaporated in vacuo to yield crude 2-(2,3 dihydrobenzo[1,4]dioxin-2-yl)ethylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08084490B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-0fdfbe23094640898f4953d00721f35f |
| 出典メモ | uspto-grants-2011_12 |