関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,2-Bis(chloromethyl)benzene | HCID 11919 | — |
| 反応物 | 1,2-Benzenedimethanol | HCID 69153 | — |
| 反応物 | [2-(Chloromethyl)phenyl]methanol | HCID 12416357 | — |
| 生成物 | 1,3-Dihydroisobenzofuran | HCID 10327 | 2% |
反応手順
A reagent, α,α′-dihydroxy-o-xylene, produced by Aldrich Co. (69.5 g, 0.5 mol) was placed in a 500-mL four-neck flask equipped with a condenser tube, a stirring blade, a thermometer, and a dropping funnel, and 35% hydrochloric acid (100 g, 1.0 mol) was added thereto. The mixture was stirred at 70° C. for one hour. After completion of reaction, the reaction mixture was allowed to stand, so that two-separated layers were formed. The reaction was analyzed through GC while stirring again during sampling. From the obtained concentration of α-chloro-α′-hydroxy-o-xylene, the yield of α-chloro-α′-hydroxy-o-xylene was calculated to be 91% based on α,α′-dihydroxy-o-xylene. The conversion of α,α′-dihydroxy-o-xylene was 99%, and α,α′-dichloro-o-xylene (5%) and phthalan (2%) were formed as by-products.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06372921B1 |
|---|
| 出典データセット | uspto-grants-2002_04 |
|---|
| ORD ID | ord-e5cb971104e741ab8a3c6cc2047f7110 |
|---|
| 出典メモ | uspto-grants-2002_04 |
|---|