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Methyl 4-aminobenzoate → Methyl 4-{[1-(5-methoxy-3-methyl-1-benzofuran-2-yl)heptyl]amino}benzoate

HRID 2091227
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HRID 2091227 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][C:9]([C:11](=O)[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[C:8]([CH3:19])[C:7]=2[CH:20]=1.[NH2:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=1.C(=O)([O-])O.[Na+].C([BH3-])#N.[Na+]>O1CCCC1.[Ti](Cl)(Cl)(Cl)Cl.C(O)(=O)C.C(Cl)Cl.C(N(CC)CC)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][C:9]([CH:11]([NH:21][C:22]3[CH:23]=[CH:24][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:30][CH:31]=3)[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[C:8]([CH3:19])[C:7]=2[CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 12082Methyl 4-aminobenzoateHCID 516892Sodium Bicarbonate2회HCID 5003444Sodium cyanoborohydrideHCID 667773831-(5-Methoxy-3-methyl-1-benzofuran-2-yl)heptan-1-one

생성물 1

HCID 66778946Methyl 4-{[1-(5-methoxy-3-methyl-1-benzofuran-2-yl)heptyl]amino}benzoate수율 66.4%

시약·촉매·용매 5

HCID 24193
Titanium Tetrachloride
촉매
HCID 176Acetic Acid용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매
HCID 8471Triethylamine용매

실험 절차

To a mixture of 1-(5-methoxy-3-methyl-1-benzofuran-2-yl)heptan-1-one (1.18 g) synthesized above, methyl 4-aminobenzoate (715 mg), triethylamine (4.79 mL) and methylene chloride (20 mL) was added titanium (IV) chloride (566 μL), and the mixture was stirred under argon atmosphere overnight at room temperature. Saturated aqueous sodium hydrogen carbonate solution was added to quench the reaction, methylene chloride was evaporated in an evaporator, and the residue was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure to give a dark brown oil. To a solution (20 mL) of the obtained oil in tetrahydrofuran were added acetic acid (1.23 mL) and sodium cyanoborohydride (540 mg), and the mixture was stirred at room temperature for 1 hr. Saturated aqueous sodium hydrogen carbonate solution was added to quench the reaction, and the reaction mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (0-20% ethyl acetate/hexane) to give the title object compound (1.17 g, 66%) as a pale-brown oil

후처리

  1. customto quench
  2. customthe reaction, methylene chloride
  3. customwas evaporated in an evaporator
  4. extractionthe residue was extracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto give a dark brown oil
  9. stirringthe mixture was stirred at room temperature for 1 hr
  10. customto quench
  11. customthe reaction
  12. extractionthe reaction mixture was extracted with ethyl acetate
  13. washThe extract was washed with saturated brine
  14. dry with materialdried over magnesium sulfate
  15. concentrationconcentrated under reduced pressure
  16. customThe residue was purified by silica gel column chromatography (0-20% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-07eabd29a062448aad66b9f423baabee
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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