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Sodium hydride → (3-Iodo-4-methyl-benzyloxy)-acetic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 反応物 | 3-Iodo-4-methylbenzyl alcohol | HCID 5166798 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (3-Iodo-4-methyl-benzyloxy)-acetic acid tert-butyl ester | HCID 69586267 | 143.6% |
反応手順
The procedure used in Example 299: step a was followed using sodium hydride (53 mg, 2.2 mmol), 3-iodo-4-methyl-benzyl alcohol (992 mg, 4 mmol), tert-butyl bromoacetate (0.4 mL, 2.5 mmol) in DMF (10 mL). Analogous aqueous workup and purification by SiO2 flash column chromatography yielded the title compound (1.30 g, 89%) as an oil. 1H-NMR (CDCl3): δ 7.84 (d, 1H, J=1.4 Hz), 7.27 (d, 1H, J=1.4 Hz), 7.23 (d, 1H, J=7.7 Hz), 4.55 (s, 2H), 3.99 (s, 2H), 2.44 (s, 3H), 1.51 (s, 9H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07109354B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-802c7583552d474c846c4d31708fcc44 |
| 出典メモ | uspto-grants-2006_09 |