Hydrochloric Acid → HCID 22990026, 화합물

HRID 1169358노트

반응식

HRID 1169358 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][CH:12]=3)[CH:9]=2)[CH:4]=[C:3]1[C:18]([O:20]CC)=[O:19].[OH-].[Na+].Cl>C(O)C.C1COCC1>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][CH:12]=3)[CH:9]=2)[CH:4]=[C:3]1[C:18]([OH:20])=[O:19]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22989974ethyl 1-methyl-6-(4-methylphenyl)-1H-indole-2-carboxylate

생성물 1

HCID 22990026HCID 22990026, 화합물수율 94.8%

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

Into a mixed solution of ethyl 1-methyl-6-(4-methylphenyl)-1H-indole-2-carboxylate (0.7 g) in ethanol/THF (20/10 ml) was added at room temperature a 2 N aqueous solution of sodium hydroxide (1.5 ml), and the resulting mixture was stirred for 24 hours. After addition of 1 N hydrochloric acid (5 ml), the reaction mixture was concentrated under reduced pressure. Water was added to the residue, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with magnesium sulfate. After concentration under reduced pressure, the precipitated crystals were collected by filtration. The crystals were washed with hexane to obtain 1-methyl-6-(4-methylphenyl)-1H-indole-2-carboxylic acid (600 mg) as colorless crystals.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. extractionthe resulting mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
  5. dry with materialwas dried with magnesium sulfate
  6. concentrationAfter concentration under reduced pressure
  7. filtrationthe precipitated crystals were collected by filtration
  8. washThe crystals were washed with hexane

출처 및 근거

ORD 기록
ord-9813251a77974c259c7fe850ea5a4ce1
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627651B1

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