関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 反応物 | 4-Iodobenzenecarbohydrazide | HCID 306104 | — |
| 生成物 | 2-(4-Iodophenyl)-5-methyl-[1,3,4]oxadiazole | HCID 676569 | — |
反応手順
Triethyl orthoacetate (10 ml) was added to 4-iodo-benzoic acid hydrazide (Intermediate 14) (0.55 g, 2.1 mmol) and heated under nitrogen at 130° C. for 3 hours. The triethyl orthoacetate was removed in vacuo and the residue partitioned between ethyl acetate (30 ml) and water (30 ml). The organic layer was washed with water (50 ml), brine (50 ml), dried over magnesium sulfate filtered and the solvent removed in vacuo. The residue was purified by silica SPE cartridge (10 g) eluting with 20:1 cyclohexane/ethyl acetate v:v to 5:1 cyclohexane/ethyl acetate v:v. The desired product was obtained as a white solid (0.31 g, 1.1 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425555B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-83ed388e738c4ac3a3d041d293b05383 |
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| 出典メモ | uspto-grants-2008_09 |
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