Water → 2H-Indol-2-one, 3-(1,3-dihydro-3-oxo-2H-indol-2-ylidene)-1,3-dihydro-

HRID 2170829

反応式

HRID 2170829 の反応式
CC([O:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)=O.[NH:14]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:17](=O)[C:15]1=[O:16].C(=O)([O-])[O-].[Na+].[Na+].O>CO>[CH:21]1[CH:22]=[CH:23][C:24]2[NH:14][C:15]([OH:16])=[C:17]([C:6]3[C:5](=[O:4])[C:13]4[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=4[N:7]=3)[C:19]=2[CH:20]=1

参加物

6

反応物 4

HCID 962WaterHCID 7054IsatinHCID 10340Sodium CarbonateHCID 11841Indoxyl acetate

生成物 1

HCID 101772H-Indol-2-one, 3-(1,3-dihydro-3-oxo-2H-indol-2-ylidene)-1,3-dihydro-収率 69%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Argon gas was blown into a suspension of indoxyl acetate (1.75 g, 10 mmol) and isatin (1.47 g, 10 mmol) in anhydrous methanol (20 mL) for 5 minutes. Sodium carbonate (2.12 g, 20 mmol) was added to the reaction liquid and stirred at room temperature for 18 hours. The reaction liquid was then poured into water (1 L). The precipitated crude crystals were collected by suction filtration. The resulting crude crystals were recrystallized from 1,4-dioxane/hexane to give purple needle-shaped crystals of indirubin (1.81 g, 69%).

後処理

  1. customThe reaction liquid
  2. customThe precipitated crude crystals
  3. filtrationwere collected by suction filtration
  4. customThe resulting crude crystals were recrystallized from 1,4-dioxane/hexane

出典と根拠

ORDレコード
ord-30cea05770bc462e902cffa231059acd
出典データセット
uspto-grants-2015_06
特許番号
US09051306B2

関連ノート

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