Sulfuric Acid → HCID 66835156、化合物

HRID 61902ノート

反応式

HRID 61902 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH:8]([C:16]3[C:21]([O:22]CC4C=CC(OC)=CC=4)=[CH:20][CH:19]=[CH:18][N:17]=3)[C:9](=O)[C:10]2([CH3:14])[CH3:13])=[CH:5][CH:4]=1.S(=O)(=O)(O)O.[OH-].[Na+]>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:7][C:8]3[C:16]4[N:17]=[CH:18][CH:19]=[CH:20][C:21]=4[O:22][C:9]=3[C:10]([CH3:14])([CH3:13])[C:11]=2[CH:12]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 66834426HCID 66834426、化合物

生成物 1

HCID 66835156HCID 66835156、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

反応条件

温度
70 °C

実験手順

To the mixture of 7-methoxy-3-[3-(4-methoxy-benzyloxy)-pyridin-2-yl]-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound GT15-2, 21 mg) and ethyl acetate (0.8 ml), sulfuric acid (0.2 ml) was added. The mixture was stirred and heated at 70° C. for 5 hrs. After cooling, the reaction mixture was neutralized with 2 N aqueous solution of sodium hydroxide. The mixture was diluted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium bicarbonate and saturated brine, and then concentrated under reduced pressure. The resulting residues were purified by silica gel column (ethyl acetate/hexane) to obtain the title compound (7 mg, 50%).

後処理

  1. additionwas added
  2. temperatureAfter cooling
  3. washThe organic layer was washed with saturated aqueous solution of sodium bicarbonate and saturated brine
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residues were purified by silica gel column (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-58611dccb4184d72b2396b5ebe6a1bc4
出典データセット
uspto-grants-2016_09
特許番号
US09440922B2

反応ノート

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