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Iodine → 2-Iodo-3-(4-methoxyphenoxy)benzo[b]thiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 3-(4-Methoxyphenoxy)benzo[b]thiophene | HCID 10824975 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Iodo-3-(4-methoxyphenoxy)benzo[b]thiophene | HCID 10691279 | — |
反応手順
A solution of 133 mg (0.52 mmol) of 3-(4-methoxyphenoxy)benzo[b]thiophene (Part A) in 3 mL of THF was treated with 0.33 mL of 1.6 M n-BuLi in hexanes (0.54 mmol) at −78° C. for 15 min and then treated with 138 mg (0.54 mmol) of I2 in 3 mL of THF. The reaction was allowed to gradually warm to room temperature and then partitioned between brine and EtOAc/hexanes. The two phases were separated, the organic phase was washed with H2O, dried over Na2SO4, and concentrated in vacuo. The residue was crystallized from hexanes to afford 143 mg (0.37 mmol; 72%) of the title compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06265575B1 |
| 出典データセット | uspto-grants-2001_07 |
| ORD ID | ord-e24f8b5bbe76440ea6c3491bd4deaad9 |
| 出典メモ | uspto-grants-2001_07 |