Hydrogen Bromide → HCID 22033294、化合物

HRID 1792314ノート

反応式

HRID 1792314 の反応式
C[O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1.Br>C(O)(=O)C>[OH:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 109799547-Methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one

生成物 1

HCID 22033294HCID 22033294、化合物収率 92.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one (2.27 g, 7.22 mmol) in acetic acid (75 ml) was added 48% aqueous HBr solution (75 mg), which was then heated under reflux for 1 day. The reaction mixture was extracted with diethyl ether. The organic layer was washed with saturated sodium bicarbonate solution and saturated saline solution, dried over anhydrous magnesium sulfate, and concentrated. Then, the residue was subjected to flash chromatography on silica gel (n-hexane:ethyl acetate=7:3 and 1:1) to give the title compound (1.92 g, yield 92%).

後処理

  1. temperaturewas then heated
  2. temperatureunder reflux for 1 day
  3. extractionThe reaction mixture was extracted with diethyl ether
  4. washThe organic layer was washed with saturated sodium bicarbonate solution and saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-1fa491b162164f098d0ec14018659b67
出典データセット
uspto-grants-2006_07
特許番号
US07074819B2

反応ノート

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