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Water → 1,3-Bis(2-chlorothiophenoyl)Benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Chlorothiophene | HCID 7299 | — |
| 反応物 | Isophthaloyl chloride | HCID 7451 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 1,3-Bis(2-chlorothiophenoyl)Benzene | HCID 67784004 | 75% |
反応手順
A solution of 2-chlorothiophene (0.128 mol) in 20 mL of carbon disulfide was added to a stirred suspension of isophthaloyl chloride (0.064 mol) and anhydrous aluminum chloride (0.1408 mol) in 100 mL of carbon disulfide. The reaction mixture was heated to reflux, stirred under nitrogen for 3 hours, and poured into 300 mL of water. The organic layer was separated immediately, then washed twice with 3.00 mL of 10% NaOH, twice with 300 mL of 5% HCl, and once with 500 mL of water. The product was recrystallized twice from ethyl acetate to form light yellow crystals in a 75% yield. Purity was determined by GC to be greater than 99.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420224 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-9e5555306d5d4ec291cd6d21577f16ab |
| 出典メモ | uspto-grants-1995_05 |