関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl phenylmalonate | HCID 66514 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Monosodium phosphate | HCID 23672064 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Phenyl-1,3-propanediol | HCID 254178 | 63% |
反応手順
Sodium dihydrogen phosphate (58.3 g) was added to a solution of 50 g of diethyl phenylmalonate in 350 ml of ethanol. The mixture was cooled to 5-7° C. and a solution of 16.7 g of sodium borohydride in 38 ml of 0.2% NaOH was gradually added. The mixture was stirred for additional 2 hours and the Ethanol was distilled out. The reaction was quenched by adding 132 ml of water followed by heating to 50° C.-60° C. for 2 hours. The solution was then basified with 50% NaOH and extracted with ethyl acetate. The organic layer was washed with water and evaporated to dryness. The precipitate was crystallized from toluene. 20 g of 2-phenyl-1,3-propanediol was obtained with a yield of 63%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09233898B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-b88aeaad75c048ccbe383ea0a0fd611f |
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| 出典メモ | uspto-grants-2016_01 |
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