関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,6-Difluorobenzyl alcohol | HCID 87921 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Acetic acid 2,6-difluorobenzyl ester | HCID 12084134 | 76% |
反応手順
Acetyl chloride (1.13 mL, 15.8 mmol) was added dropwise to a solution of 2,6-difluorobenzyl alcohol (1.76 g, 12.2 mmol) and triethylamine (3.43 mL, 24.4 mmol) in DCM (20 mL) at 0° C. The reaction mixture was stirred at 0° C. for 30 min. The reaction mixture was diluted with water and extracted with DCM (3×20 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, eluting with 0-100% EtOAc in cyclohexane) to yield the title compound as a colourless oil (1.72 g, 76%). 1H NMR 400 MHz δ (CDCl3): 7.37-7.28 (1H, m), 6.96-6.88 (2H, m), 5.20 (2H, s), 2.08 (3H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653089B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-1d6104a333ff4c25aed6fda04fe7a4c2 |
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| 出典メモ | uspto-grants-2014_02 |
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