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Methanol → HCID 66726052, 화합물

HRID 1042141
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HRID 1042141 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([O:16][C:17]2[CH:18]=[N:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=2)[CH:5]=[C:6]2[C:10]=1[NH:9][C:8]([C:11]([O:13]CC)=[O:12])=[CH:7]2.CO.[OH-].[K+]>O1CCCC1>[CH3:1][C:2]1[CH:3]=[C:4]([O:16][C:17]2[CH:18]=[N:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=2)[CH:5]=[C:6]2[C:10]=1[NH:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 66726116HCID 66726116, 화합물

생성물 1

HCID 66726052HCID 66726052, 화합물수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 7-methyl-5-{[6-(methylsulfonyl)pyridin-3-yl]oxy}-1H-indole-2-carboxylate (3.9 g), methanol (30 mL), and tetrahydrofuran (50 mL) was added aqueous solution (20 mL) of potassium hydroxide (2.0 g), and the mixture was stirred at room temperature for 15 hr. The reaction solution was concentrated, acidified with aqueous citric acid solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained pale-yellow crystals were washed with ethyl acetate-hexane to give the title compound (3.30 g, yield 92%) as pale-yellow crystals.

후처리

  1. concentrationThe reaction solution was concentrated
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. washThe obtained pale-yellow crystals were washed with ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-b32b27ac7d3246c0951df7796460eebc
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08557805B2

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