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Triethylamine → tert-butyl 2-(2-bromo-4-((3-chloro-4-fluoro-N-methylphenylsulfonamido)methyl)phenoxy)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Chloro-4-fluorobenzenesulphonyl chloride | HCID 145222 | — |
| 反応物 | t-Butyl 2-(2-bromo-4-((methylamino)methyl)phenoxy)acetate | HCID 66868764 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-butyl 2-(2-bromo-4-((3-chloro-4-fluoro-N-methylphenylsulfonamido)methyl)phenoxy)acetate | HCID 67527857 | 59% |
反応手順
To a solution of t-butyl 2-(2-bromo-4-((methylamino)methyl)phenoxy)acetate (2) (68.8 g, 0.21 mol, 1 eq) in DCM (500 mL) was added triethylamine (42 g, 0.42 mol, 2 eq) and 3-chloro-4-fluorobenzene-1-sulfonyl chloride (47.8 g, 0.21 mol. 1 eq, Aldrich, Milwaukee, Wis., USA). After the mixture was stirred for 2 h at room temperature, DCM was evaporate. Crude product was recrystallized from ethanol to yield tert-butyl 2-(2-bromo-4-((3-chloro-4-fluoro-N-methylphenylsulfonamido)methyl)phenoxy)acetate (10) (64 g, 59%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822467B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-fbe159645fc842e3ada662ef177bc857 |
| 出典メモ | uspto-grants-2014_09 |