関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Benzoic acid, 2-amino-5-iodo- | HCID 72911 | — |
| 反応物 | 1,1,1-Trifluoro-3-phenyl-2-propanone | HCID 222958 | — |
| 反応物 | Phosphorus Pentoxide-Methanesulfonic Acid | HCID 86584057 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178515324 | HCID 178515324 | — |
反応手順
A mixture of 2-amino-5-iodobenzoic acid (5.20 g, 19.8 mmol), 1,1,1-trifluoro-3-phenylpropan-2-one (3.95 g, 21.0 mmol), and Eaton's reagent (12 mL) in a sealed tube was heated at 100° C. for 2 hours. More 1,1,1-trifluoro-3-phenylpropan-2-one (1.60 g, 8.50 mmol) was added and the mixture was heated for another 2 hours. The reaction was then cooled to room temperature, ice water was added, and the mixture was stirred vigorously for about 20 min. 50% NaOH and conc. NH4OH solution were added until pH was 9. Some gummy dark brown material formed. After the addition of CH2Cl2, the gummy material became fluffy solid. This solid was filtered, washed with water and Et2O, and air dried to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09309222B2 |
|---|
| 出典データセット | uspto-grants-2016_04 |
|---|
| ORD ID | ord-1929ab8ba3eb4739a08d589c4e9fc9ad |
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| 出典メモ | uspto-grants-2016_04 |
|---|
