Hydrochloric Acid → 4-(5-Bromothiazol-2-yl)-4-hydroxycyclohexanone
反応式
[Br:1][C:2]1[S:6][C:5]([C:7]2([OH:17])[CH2:16][CH2:15][C:10]3(OCC[O:11]3)[CH2:9][CH2:8]2)=[N:4][CH:3]=1.Cl.CCOC(C)=O.O>C1COCC1>[Br:1][C:2]1[S:6][C:5]([C:7]2([OH:17])[CH2:8][CH2:9][C:10](=[O:11])[CH2:15][CH2:16]2)=[N:4][CH:3]=1参加物
6
実験手順
The product of Step 1 (3.0 g, 9.4 mmol) was dissolved in 30 mL of 1:1 THF:HCl (3N) and heated at 50° C. for 8 hours and the solution neutralized with solid KHCO3 and then EtOAc (100 mL) and water (20 mL) were added. The aqueous layer was then extracted with EtOAc (50 mL) and the combined organic layers were washed with brine (50 mL), evaporated to a slurry which was treated with hexanes (20 mL). Filtration and drying afforded 4-(5-bromo-1,3-thiazol-2-yl)-4-hydroxycyclohexanone as a white solid (2.1 g, 7.7 mmol).
後処理
- extractionThe aqueous layer was then extracted with EtOAc (50 mL)
- washthe combined organic layers were washed with brine (50 mL)
- customevaporated to a slurry which
- additionwas treated with hexanes (20 mL)
- filtrationFiltration
- customdrying
出典と根拠
- ORDレコード
- ord-c730726318244cf785bf4f91c9056fb2
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759366B2
反応ノート
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