関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Acetyl-5-bromothiophene | HCID 79335 | — |
| 反応物 | Tetrahydrofuran toluene | HCID 22635083 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Bromo-alpha,alpha-dimethyl-2-thiophenemethanol | HCID 22714302 | — |
反応手順
To a solution of 2-acetyl-5-bromothiophene in THF (2.5 mL/mmol) at −30° C. was added 1.4M methylmagnesium bromide in 3:1 toluene-THF (1.5 eq) and the resulting mixture was warmed to −10° C. and stirred for 1.5 hours. After quenching with saturated aqueous ammonium chloride solution, the mixture was partitioned between ether and water. The organic fraction was dried and evaporated, and the crude material was chromatographed on silica gel eluting with a 1:4 mixture of ether and hexane to afford the 2-bromo-5-(1-hydroxy-1-methylethyl)thiophene compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06743802B2 |
|---|
| 出典データセット | uspto-grants-2004_06 |
|---|
| ORD ID | ord-1e0a865ae353492d95932dc9687937af |
|---|
| 出典メモ | uspto-grants-2004_06 |
|---|