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Methanol → 1-(4-Methoxybutyl)-3,3-dimethyl-2-oxoindoline-6-carboxylic acid

HRID 1942538
ノート
印刷プレビュー

反応式

HRID 1942538 の反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:16]([O:18]C)=[O:17])[CH:14]=2)[C:9]([CH3:21])([CH3:20])[C:8]1=[O:22].[OH-].[Na+].CO>C1COCC1>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:16]([OH:18])=[O:17])[CH:14]=2)[C:9]([CH3:20])([CH3:21])[C:8]1=[O:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 67330620Methyl 1-(4-methoxybutyl)-3,3-dimethyl-2-oxoindoline-6-carboxylate

生成物 1

HCID 673310081-(4-Methoxybutyl)-3,3-dimethyl-2-oxoindoline-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

To methyl 1-(4-methoxybutyl)-3,3-dimethyl-2-oxoindoline-6-carboxylate (480 mg) were added 2N aqueous NaOH solution (5 ml), MeOH (5 ml), and THF (5 ml), and the mixture was stirred at 65° C. for one hour. After the reaction was complete, the solvent was concentrated, and to the resultant was added dropwise 2N aqueous hydrochloric acid solution. The precipitated crystals were extracted with ethyl acetate, and this ethyl acetate solution was washed with water and an aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated. The obtained residue (400 mg) was used in the subsequent reaction without further treatment.

後処理

  1. concentrationthe solvent was concentrated
  2. additionto the resultant was added dropwise 2N aqueous hydrochloric acid solution
  3. extractionThe precipitated crystals were extracted with ethyl acetate
  4. washthis ethyl acetate solution was washed with water
  5. dry with materialan aqueous sodium chloride solution, dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe obtained residue (400 mg) was used in the subsequent reaction without further treatment

出典と根拠

ORDレコード
ord-910e1a4e7a7f408c97c4b501b9c5980e
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08389511B2

反応ノート

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