Potassium Carbonate → HCID 90229320、化合物
反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(=O)([O-])[O-].[K+].[K+].I[CH2:20][CH:21]([F:23])[F:22]>CC(C)=O>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH2:20][CH:21]([F:23])[F:22])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]参加物
5
実験手順
To a suspension of methyl 2-chloro-5-hydroxybenzoate (50 mg) and potassium carbonate (111 mg) in acetone (1 mL) was added 2-iodo-1,1-difluoroethane (35 μL), and the suspension was reacted at 120° C. for 10 minutes in a microwave synthesizer (Biotage, Initiator). After reaction at 130° C. for additional 15 minutes, the reaction mixture was directly purified on silica gel column chromatography to obtain the titled compound (55 mg) as yellow oil.
後処理
- customthe suspension was reacted at 120° C. for 10 minutes in a microwave synthesizer (Biotage, Initiator)
- customAfter reaction at 130° C. for additional 15 minutes
- customthe reaction mixture was directly purified on silica gel column chromatography
出典と根拠
- ORDレコード
- ord-5e3bed580f5946c9a5757d95a2858363
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216968B2
反応ノート
読み込み中…