関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 4-(2-Chloroethylthio)benzoic acid | HCID 18316694 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 13394557 | HCID 13394557 | — |
反応手順
4-(2-Chloroethylsulfanyl)-benzoic acid (18.4 mmol) is suspended in methylene chloride (60 ml) and cooled to −10C. m-Chloroperbenzoic acid (38.6 mmol) are added dropwise in methylene chloride (60 ml) and the mixture is stirred for e hours at −10° C. The mixture is diluted methylene chloride (100 ml) and a 5% solution of sodium thiosulfate in water is added and the mixture vigorously stirred. The mixture is extracted, washed with water and and dried over sodium sulfate and evaporated. The crude product is recrystallized from ethylacetate and the solid filtered of and dried (vacuum). 2.19 g of a pale powder with mp. 142-144° C., Rf=0.37 (CH2Cl2/MeOH=9:1) is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06353017B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-e28ffb9f082942739d856da13297091f |
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| 出典メモ | uspto-grants-2002_03 |
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