Citric Acid → HCID 57901602, 화합물

HRID 1851490노트

반응식

HRID 1851490 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([NH:12][S:13]([C:16]3[S:17][CH:18]=[CH:19][CH:20]=3)(=[O:15])=[O:14])[CH:11]=1)[NH:8][C:7]([C:21]([O:23]CC)=[O:22])=[CH:6]2.CO.[OH-].[K+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([NH:12][S:13]([C:16]3[S:17][CH:18]=[CH:19][CH:20]=3)(=[O:15])=[O:14])[CH:11]=1)[NH:8][C:7]([C:21]([OH:23])=[O:22])=[CH:6]2

참가 물질

6

반응물 4

HCID 311Citric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 57901653HCID 57901653, 화합물

생성물 1

HCID 57901602HCID 57901602, 화합물수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixed solution of ethyl 5-methoxy-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (0.34 g) in tetrahydrofuran (10 mL)-methanol (10 mL) was added aqueous solution (5 mL) of 85% potassium hydroxide (0.20 g), and the mixture was stirred at room temperature for 15 hr. Aqueous citric acid solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were washed with ethyl acetate-hexane to give the title compound (300 mg, yield 96%) as pale-yellow crystals. melting point>240° C. (decomposition).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washThe obtained crystals were washed with ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-029eeebeb4e3404cb3a5025de3d214d9
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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