4-Chloro-3-methylphenol → HCID 22467254、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[CH3:9].C([O-])([O-])=O.[K+].[K+].Br[CH2:17][CH2:18][O:19][CH3:20]>CN(C=O)C.O.CCOCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:17][CH2:18][O:19][CH3:20])=[CH:4][C:3]=1[CH3:9]参加物
7
実験手順
To a stirred solution of 4-chloro-3-methylphenol (1 eq.) in DMF (0.7 M) was added K2CO3 (1.2 eq.). The mixture was stirred at 50° C. for 5 min before 1-bromo-2-methoxyethane (1.5 eq.) was added. After 2 h at 70° C., the reaction mixture was cooled down to RT and then diluted with water and ether. The organic phase was separated and washed sequentially with 2 N aq. NaOH, water and brine. The organic extract was dried over Na2SO4, filtered and the filtrate concentrated in vacuo to afford the title compound as a yellowish oil.
後処理
- additionwas added
- customThe organic phase was separated
- washwashed sequentially with 2 N aq. NaOH, water and brine
- extractionThe organic extract
- dry with materialwas dried over Na2SO4
- filtrationfiltered
- concentrationthe filtrate concentrated in vacuo
出典と根拠
- ORDレコード
- ord-ce8696ec85d046e4b4bc07a5a4c1936d
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08889714B2
反応ノート
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