関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester | HCID 67843 | — |
| 反応物 | tert-Butyl 5-hydroxy-1,3-dihydro-2H-isoindole-2-carboxylate | HCID 18630963 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Difluoromethoxy-1,3-dihydro-isoindole-2-carboxylic acid tert-butyl ester | HCID 57753212 | 40% |
反応手順
A mixture containing 0.68 mmol 5-Hydroxy-1,3-dihydro-isoindole-2-carboxylic acid tert-butyl ester (CAS: 226070-47-9), 0.68 mmol potassium carbonate and 0.68 mmol ethyl chlorodifluoroacetate in 1.5 ml DMF was stirred overnight at 65° C. The mixture was then partitioned between ethyl acetate and water and the organic phase was then separated, dried over sodium sulfate, and concentrated in vacuo. The residue was purified by chromatography on silica gel (eluant: n-heptane/ethylacetate) to afford the title compound as a white solid (40% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07557114B2 |
|---|
| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-7eeace9b5415458084a6e8d730a81053 |
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| 出典メモ | uspto-grants-2009_07 |
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