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Potassium Carbonate → HCID 67428163, 화합물

HRID 1662628
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HRID 1662628 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2([CH2:20][C:21]([OH:23])=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[O:18][CH3:19].C1C=CC2N(O)N=NC=2C=1.O.C(Cl)CCl.Cl.[N:40]1([C:46]2[N:51]=[CH:50][CH:49]=[CH:48][N:47]=2)[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O.CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[O:18][CH3:19])[CH2:20][C:21](=[O:23])[N:43]1[CH2:44][CH2:45][N:40]([C:46]2[N:47]=[CH:48][CH:49]=[CH:50][N:51]=2)[CH2:41][CH2:42]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 11430Potassium CarbonateHCID 887471-(2-Pyrimidinyl)piperazineHCID 27960291-Hydroxybenzotriazole hydrateHCID 21925457HCID 21925457, 화합물HCID 22619321HCID 22619321, 화합물

생성물 1

HCID 67428163HCID 67428163, 화합물수율 94.6%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 800 mg of [5-chloro-3-(2-methoxyphenyl)-2-oxo-2,3-dihydro-1H-indol-3-yl]acetic acid, which is the compound described in Preparation 1.1 of the brochure WO03/008407 and 488 mg of HOBt/H2O in DMF (8 ml) was added 554 mg of EDC/HCl under ice cooling, then, the reaction mixture was warmed to room temperature and stirred at room temperature for 30 minutes. The solution was cooled with ice again, 433 mg of 2-piperazin-1-yl pyrimidine was added to the reaction solution, and after warming to room temperature, the reaction mixture was stirred at room temperature for 14 hours. To the reaction solution was added EtOAc, a saturated aqueous solution of K2CO3 and water, and the mixture was stirred for 30 minutes. Liquid separation was performed, the obtained aqueous layer was extracted with EtOAc, the combined organic layer was washed with water and saturated brine, then, was dried over MgSO4, the drying agent was separated by filtration, then the solvent was evaporated under reduced pressure. The obtained residue was subjected to column chromatography (silicagel 60; mobile phase: CHCl3/MeOH/OH=10/1/0.1; v/v/v) to obtain 1.09 g of the title compound (colorless solid).

후처리

  1. temperatureThe solution was cooled with ice again
  2. temperatureafter warming to room temperature
  3. stirringthe reaction mixture was stirred at room temperature for 14 hours
  4. customLiquid separation
  5. extractionthe obtained aqueous layer was extracted with EtOAc
  6. washthe combined organic layer was washed with water and saturated brine
  7. dry with materialwas dried over MgSO4
  8. customthe drying agent was separated by filtration
  9. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f059cd3530fd427d844483f5a1943187
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030499B2

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