関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromoaniline | HCID 11992 | — |
| 反応物 | Diphenylmaleic anhydride | HCID 78530 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(2-Bromoanilino)-2,3-diphenyl-4-hydroxybutyrolactone | HCID 86590036 | 40% |
反応手順
A mixture of 2-bromoaniline (2.18 g, 12.7 mmol) and 2,3-diphenylmaleic anhydride (3.17 g, (12.7 mmol) were stirred and heated under argon to 200° C. for 6 h. The mixture was cooled to room temperature, dissolved in CH2Cl2 (50 mL), dried (MgSO4) and evaporated. Purification of the crude product by flash chromatography on silica gel (5×25 cm column, 2 L of 3:7 hexanes/CH2Cl2, then CH2Cl2) gave first 4-(2-bromoanilino)-2,3-diphenyl-4-hydroxybutyrolactone (2.16 g, 40% yield) as a yellow solid, mp 162-164° C. and then the title compound as a bright yellow solid, mp 178-180° C., 2.00 g, 39% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06927227B2 |
|---|
| 出典データセット | uspto-grants-2005_08 |
|---|
| ORD ID | ord-c40effe431974020971c577d1d017b0f |
|---|
| 出典メモ | uspto-grants-2005_08 |
|---|