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Nitrogen → 4-(3-Bromo-phenylsulfanylmethyl)-2-phenyl-thiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | m-Bromobenzenethiol | HCID 80597 | — |
| 反応物 | 4-(Chloromethyl)-2-phenyl-1,3-thiazole | HCID 236969 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3-Bromo-phenylsulfanylmethyl)-2-phenyl-thiazole | HCID 59654608 | — |
反応手順
NaH (53 mg, 2.2 mmol) was suspended in dry THF (1.5 ml) under a stream of N2 and 3-bromo-benzenethiol (378 mg, 2 mmol) was added dropwise to the suspension over 5 min. 4-Chloromethyl-2-phenyl-thiazole (419 mg, 2 mmol) was added and the solution left stirring overnight. The reaction mixture was quenched with a saturated K2CO3 solution (8 ml) and extracted with EtOAc (3×4 ml). The combined organic layers were washed with saturated K2CO3 solution (4 ml), dried (MgSO4), filtered and the solvent removed in vacuo. The residue was purified by column chromatography eluting with 20% EtOAc in heptane to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07662839B2 |
| 出典データセット | uspto-grants-2010_02 |
| ORD ID | ord-0663b778deaf40fb8b34e07164706c1e |
| 出典メモ | uspto-grants-2010_02 |