Triethylamine → HCID 12894082、化合物
反応式
[CH3:1][O:2][CH:3]1[O:8][CH2:7][C:6](=[O:9])[CH:5]=[CH:4]1.[Br:10]Br.C(N(CC)CC)C>C(Cl)Cl.C1(C)C=CC=CC=1>[Br:10][C:5]1[C:6](=[O:9])[CH2:7][O:8][CH:3]([O:2][CH3:1])[CH:4]=1参加物
6
実験手順
To a solution of 6-methoxy-2H-pyran-3(6H)-one 12.8 (0.1 mole) in 40 ml CH2Cl2 at 0° C. was added 16.0 g (0.1 mole) of bromine in 10 ml of CH2Cl2. Then 14 ml of triethylamine was added dropwise at 0° C. and the reaction was allowed to warm to room temperature and stir for two hours. The reaction was then diluted with 200 ml of toluene. After filtration, the organic solution was then washed with 5% NaHCO3 and brine, dried with Na2SO4, filtered and concentrated to yield the crude product as light brown solid Recrystallisation from ethyl acetate afforded the title compound (17 g, 82%) as a white crystalline solid. m.p. 74-75° C.
後処理
- filtrationAfter filtration
- washthe organic solution was then washed with 5% NaHCO3 and brine
- dry with materialdried with Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customto yield
- customthe crude product as light brown solid Recrystallisation from ethyl acetate
出典と根拠
- ORDレコード
- ord-6e6bc1b1fd294dc9a1d69a9c3d4a4639
- 出典データセット
- uspto-grants-2003_01
- 特許番号
- US06506911B2
反応ノート
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