関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (1,1'-Biphenyl)-4-methanol | HCID 19186 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Benzeneacetic acid, 4-hydroxy-, methyl ester | HCID 518900 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-(4-biphenylylmethoxy)phenylacetate | HCID 18508368 | 77.5% |
反応手順
A solution of 4-biphenylmethanol (800 g) in DMF (2.4 l) as cooled to 0° C and thionyl chloride (380 ml) was added to the solution for 40 min. The temperature of the reaction mixture was raised to 30±2° C. and stirring was continued for additional one hr. Methyl 4-hydroxyphenylacetate (722 g) was added and stirring was continued for 20 min at this temperature. 28% Sodium methoxide (2.93 kg) was added to the solution for 70 min and stirring was continued for 6 hr while the temperature of the reaction mixture was maintained at 50±2° C. Water (3.21) was added to the reaction mixture for 25 min while the temperature of the reaction mixture was maintained at 50±2° C. which was stirred for additional one hr at same temperature and cooled to room temperature. The precipitate was collected by filtration and washed with methanol (1.6 l) and water (6.41) sequentially to obtain the titled compound (1119 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06586475B1 |
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| 出典データセット | uspto-grants-2003_07 |
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| ORD ID | ord-b1c150ed45154311ab6003e15d80112f |
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| 出典メモ | uspto-grants-2003_07 |
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