反応式
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([O:14]C)=[O:13].O>[OH-].[Na+].CC(O)C>[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[CH2:10][CH2:11][C:12]([OH:14])=[O:13]参加物
5
実験手順
Methyl 3-(2-bromo-3,5-difluorophenyl)propanoate (prepared as described in Step 1, 4.3 g) in aqueous NaOH (4 M, 13.5 mL) and 2-propanol (30 mL) is heated at 50° C. for 2 hours. Water is added, the mixture washed with diethyl ether, acidified to ca. pH 5 by adding concentrated aqueous HCl, and extracted twice with diethyl ether. The combined extracts of the acidified mixture are washed with brine and volatiles evaporated under reduced pressure. The resulting material (Yield 3.6 g) is used in the next step without further purification. LC (METHOD 7): tR=0.99 min.
後処理
- washthe mixture washed with diethyl ether
- additionby adding concentrated aqueous HCl
- extractionextracted twice with diethyl ether
- washThe combined extracts of the acidified mixture are washed with brine and volatiles
- customevaporated under reduced pressure
- customThe resulting material (Yield 3.6 g) is used in the next step without further purification
出典と根拠
- ORDレコード
- ord-c0c3a2f4b8794fad9273437e85495432
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09308194B2
関連ノート
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