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Diethyl Ether → 2-[1,3-Dithian-2-yl]-5-nitrobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2-[1,3-Dithian-2-yl]-5-nitrobenzyl alcohol | HCID 13530283 | — |
| 反応物 | HCID 178418287 | HCID 178418287 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[1,3-Dithian-2-yl]-5-nitrobenzaldehyde | HCID 13530284 | — |
反応手順
To a solution of 3.47 g (12.8 mmol) of the Compound 3c in methylene chloride (100 mL) was added pyridinium chlorochromate (4.15 g, 19.2 mmol). The mixture was stirred for one hour, an additional pyridinium chlorochromate (2.0 g) was added, and the mixture was stirred 15 hours. Diethyl ether (200 mL) was added to the reaction mixture, and the solvent was decanted and evaporated. The residue was purified by chromatography (silica gel, chloroform) to afford the Compound 3d as light yellow crystals; m.p. 99°-101° C.; IR 1730 cm-1 (C=O); 1H NMR δ1.7-2.3 (m,2H, --CH2CH2CH2 --), 2.8-3.3 (m, 4H,--CH2CH2CH2 --), 6.13(s, 1H, --SCHS--), 7.8-8.7 (m,--3H, ArH), 10.45 (s, 1H,CHO).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04590276 |
| 出典データセット | uspto-grants-1986_05 |
| ORD ID | ord-99d47585a5764194bb543df3f1243001 |
| 出典メモ | uspto-grants-1986_05 |