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Acetic Anhydride → 4-(1-(N-Acetylamino)cyclopropyl)anisole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(4-Methoxyphenyl)cyclopropan-1-amine | HCID 12523671 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chlorine | HCID 24526 | — |
| 生成物 | 4-(1-(N-Acetylamino)cyclopropyl)anisole | HCID 19066431 | 80.1% |
反応手順
To a stirred suspension of Compound 7 (1.25 g, 7.66 mmol) in CH2 Cl2 (40 ml) was added acetic anhydride (860 mg, 8.42 mmol) and triethylamine (2.32 g, 22.98 mmol) at room temperature. The reaction mixture was stirred at room temperature for 22 h. The mixture was diluted with H2O (50 ml) and stirred for 10 min. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined solution was washed with 10% HCl aq., sat. NaHCO3 aq. and brine, dried (MgSO4) and concentrated in vacuo to give crude product (1.58 g, quant.), which was recrystallized from hexane-ethyl acetate to give Compound 8 (1.26 g, 80%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05789423 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-94aacddcb9e94717af2bf698367018a5 |
| 出典メモ | uspto-grants-1998_08 |