関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzenethiol, 2-(1-methylethyl)- | HCID 96003 | — |
| 反応物 | 3-(4-Chloro-3-nitrophenyl)acrylic acid | HCID 614919 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2-Isopropylphenyl)[2-nitro-4-(E-(carboxy)ethenyl)phenyl]sulfide | HCID 11759679 | — |
反応手順
To a stirred mixture of 4-chloro-3-nitrocinnamic acid (500 mg, 2.2 mmol) in 5 mL of anhydrous DMF with K2CO3 (911 mg, 6.6 mmol) was added 2-isopropylbenzenethiol (372 mL, 2.2 mmol) in 1 mL of DMF dropwise. The resulting mixture was then heated at 70° C. under nitrogen atmosphere over night. Water (25 mL) was then added and the reaction mixture was acidified to pH=4 with 3N HCl. The cloudy mixture was extracted with EtOAc (2×20 mL). The combined organic layer was washed with brine, dried over Na2SO4, concentrated in vacuo to give the title compound as viscous light-yellow oil, which was used for coupling with further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06867203B2 |
|---|
| 出典データセット | uspto-grants-2005_03 |
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| ORD ID | ord-7731277eb6d04191b60d745a5a719fa9 |
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| 出典メモ | uspto-grants-2005_03 |
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