関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (4-Chlorophenyl)acetic acid | HCID 15880 | — |
| 反応物 | 1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine | HCID 547712 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (4-Chlorophenyl)acetic acid tert-butyl ester | HCID 13380183 | 30.4% |
反応手順
To a suspension of N,N-dimethyl-formamide-di-tert-butyl acetal (25 ml, 104.4 mmol) in dry toluene (90 ml) was added p-chlorophenyl acetic acid (5.94 g, 34.8 mmol) and the whole heated at 80° C. for 1 h. The mixture was diluted with EtOAc (50 ml) and washed with water (50 ml), 3% aqueous NaHCO3 solution (50 ml) and brine (20 ml) and then dried over MgSO4 and evaporated to give an oil. This oil was purified using 35%, then 50% DCM in pentane to give the title product (2.4 g, 30%); 1HNMR (400 MHz, CDCl3) δ: 1.42 (s, 9H), 3.44 (s, 2H), 7.20 (d, 2H), 7.28 (d, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06849649B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-701d47aedcc34c7e947611658d0fc50a |
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| 出典メモ | uspto-grants-2005_02 |
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