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1,4-Dioxane → HCID 57479120, 화합물

HRID 556486
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HRID 556486 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][CH:7]=1.Br[C:14]1([CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=2)[C:22]2[C:17](=[CH:18][C:19]([Cl:23])=[CH:20][CH:21]=2)[NH:16][C:15]1=[O:24].O1CCOCC1>C([O-])([O-])=O.[K+].[K+]>[Cl:23][C:19]1[CH:18]=[C:17]2[C:22]([C:14]([N:8]([CH2:9][C:10]([OH:12])=[O:11])[C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=3)([CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=3)[C:15](=[O:24])[NH:16]2)=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 312751,4-DioxaneHCID 3780319(3-Chloroanilino)acetic acidHCID 575072733-Bromo-6-chloro-3-(3-chloro-benzyl)-1,3-dihydro-indol-2-one

생성물 1

HCID 57479120HCID 57479120, 화합물수율 37.1%

시약·촉매·용매 1

HCID 11430Potassium Carbonate용매

실험 절차

At room temperature, (3-Chloro-phenylamino)-acetic acid (1.25 g, 6.8 mmol) was dissolved in 10 ml 1N K2CO3 aqueous solution, then 3-Bromo-6-chloro-3-(3-chloro-benzyl)-1,3-dihydro-indol-2-one (2.5 g, 6.8 mmol) and 10 ml 1,4-dioxane were added slowly. After stirred for about 3 h, the solution was concentrated and the water layer was extracted with CH2Cl2. The organic layer was dried, concentrated to obtain the crude product and the crude product was purified by chromatography to obtain 1.2 g yellow solid rac-[[6-Chloro-3-(3-chloro-benzyl)-2-oxo-2,3-dihydro-1H-indol-3-yl]-(3-chloro-phenyl)-amino]-acetic acid.

후처리

  1. concentrationthe solution was concentrated
  2. extractionthe water layer was extracted with CH2Cl2
  3. customThe organic layer was dried
  4. concentrationconcentrated
  5. customto obtain the crude product
  6. customthe crude product was purified by chromatography

출처 및 근거

ORD 기록
ord-754096abfd684783b832a8269d148724
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058269B2

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