化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → Phenyl (3-chloro-4-(trifluoromethyl)phenyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 3-Chloro-4-(trifluoromethyl)aniline | HCID 67962 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Phenyl (3-chloro-4-(trifluoromethyl)phenyl)carbamate | HCID 57656832 | — |
反応手順
Phenyl chloroformate (0.86 mL) was added slowly to a stirring solution of 3-chloro-4-trifluoromethyl aniline (933 mg) in THF (10 mL) containing pyridine (1.07 mL) under an argon atmosphere. The reaction was stirred for 18 h then diluted with ethyl acetate (35 mL) and 1M HCl (20 mL). The organic layer was separated and washed with saturated aqueous NaHCO3 then dried (MgSO4), filtered and evaporated. Trituration with 1:9 EtOAc:isohexanes (10 mL) at reflux followed by cooling to RT afforded a solid which was filtered to afford 1.15 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07906645B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-38f70e8d280643899a052228c14cb32f |
| 出典メモ | uspto-grants-2011_03 |