Sulfuric Acid → HCID 66835156, 화합물

HRID 61902노트

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HRID 61902 반응식
[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

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 66834426HCID 66834426, 화합물

생성물 1

HCID 66835156HCID 66835156, 화합물수율 50%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

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온도
70 °C

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-58611dccb4184d72b2396b5ebe6a1bc4
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440922B2

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