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Acetic Anhydride → 5-Iodo-1-methyl-3,4-dihydroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-(2-Iodophenyl)ethanamine | HCID 10514616 | — |
| 反応物 | N-(2-iodophenethyl)acetamide | HCID 86711313 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-Iodo-1-methyl-3,4-dihydroisoquinoline | HCID 86711315 | — |
反応手順
N-(2-iodophenethyl)acetamide. A solution of 2-(2-iodophenyl)ethanamine (13.5 g, 54.6 mmol) and Ac2O (10.3 mL, 109 mmol) in 1,4-dioxane (200 mL) was heated to 100° C. for 45 min. The reaction was then allowed to cool to RT and concentrated in vacuo. The resulting residue was taken up in DCM and washed with a saturated aq. solution of NaHCO3— gas formation! The organic phase was separated, dried over Na2SO4, filtered and concentrated in vacuo to give the title compound as a yellow oil (16.2 g) which was used as it is in the next step. UPLC-MS: MS 290.3 (M+H+); UPLC rt 0.96 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08853203B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-ed8a50e664244039ad822f31729a0b9c |
| 出典メモ | uspto-grants-2014_10 |