Hydrochloric Acid → HCID 22990026、化合物

HRID 1169358ノート

反応式

HRID 1169358 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 22990026HCID 22990026、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9813251a77974c259c7fe850ea5a4ce1
出典データセット
uspto-grants-2003_09
特許番号
US06627651B1

反応ノート

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