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Tetra-n-butylammonium tribromide → 2,6-Dichloro-3-bromo-4-aminobenzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetra-n-butylammonium tribromide | HCID 23500184 | — |
| 反応物 | Methyl 4-amino-2,6-dichlorobenzoate | HCID 51341879 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,6-Dichloro-3-bromo-4-aminobenzoic acid methyl ester | HCID 54343023 | 139.4% |
反応手順
To a solution of 2,6-dichloro-4-aminobenzoic acid methyl ester (2.80 g) in CH2Cl2 (20 mL) at −10° C. was added a solution of tetrabutylammonium tribromide (6.94 g) in CH2Cl2 (30 mL) dropwise at −10° C. After 2 h, the mixture was warmed to room temperature, washed with satd. NaHCO3 and brine, dried (Na2SO4), filtered, and concentrated. The residue was purified by column chromatography (silica gel; eluent: EtOAc/hexane 1:4) to yield 2,6-dichloro-3-bromo-4-aminobenzoic acid methyl ester (2.99 g) ESMS: m/z 298 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06855843B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-dbc596b7032f48c9b0d9fb4f579b2e8c |
| 出典メモ | uspto-grants-2005_02 |