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

HRID 2170829노트

반응식

HRID 2170829 반응식
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

참가 물질

6

반응물 4

HCID 962WaterHCID 7054IsatinHCID 10340Sodium CarbonateHCID 11841Indoxyl acetate

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-30cea05770bc462e902cffa231059acd
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051306B2

반응 노트

불러오는 중…