Potassium Carbonate → 2-(2,4-Difluorophenyl)oxirane
反応式
[BH4-].[Na+].Br[CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[F:14])=[O:6].C([O-])([O-])=O.[K+].[K+]>CO>[F:14][C:8]1[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=1[CH:5]1[CH2:4][O:6]1参加物
5
実験手順
Sodium borohydride (0.367 g, 10.85 mmol) was added to a stirred solution of 2-bromo-2′,4′-difluoroacetophenone ([CAS 102429-07-2], 5.1 g, 21.7 mmol) in MeOH (152 mL) at 10° C. The mixture was stirred at RT for 1 h. Then, K2CO3 (4.499 g, 32.55 mmol) was added and the mixture was stirred at RT for 1 h. The mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. The residue was treated with water and extracted with CH2Cl2/THF. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield I-19 (2.24 g, 66%) as a yellow oil.
後処理
- stirringthe mixture was stirred at RT for 1 h
- filtrationThe mixture was filtered through diatomaceous earth
- concentrationthe filtrate was concentrated in vacuo
- additionThe residue was treated with water
- extractionextracted with CH2Cl2/THF
- customThe organic layer was separated
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customthe solvents evaporated in vacuo
- customto yield I-19 (2.24 g, 66%) as a yellow oil
出典と根拠
- ORDレコード
- ord-cda5a70adcba496dbcc8fc946b69d1c3
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08993591B2
反応ノート
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