関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 反応物 | 3-Iodo-4-methylbenzohydrazide | HCID 59732500 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(3-Iodo-4-methylphenyl)-5-methyl-1,3,4-oxadiazole | HCID 58170497 | 78.4% |
反応手順
A stirred mixture of 3-iodo-4-methylbenzohydrazide (preparation 55b, 5.00 g, 18.1 mmol) and triethyl orthoacetate (11.00 mL, 58.2 mmol) in acetic acid (30 mL) were heated to 150° C. in a sealed tube. After 3 hours, the mixture was cooled and concentrated in vacuo. Aqueous sodium hydrogen carbonate solution was added and the mixture was extracted with dichloromethane. The organic solution was dried (MgSO4) and the solvent was removed in vacuo. The crude material was purified by flash chromatography (2:1 hexanes/ethyl acetate) to give the title compound (4.26 g, 78%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08772288B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-a59ed7b6760e45f59b06d99d623f4516 |
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| 出典メモ | uspto-grants-2014_07 |
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