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Potassium Carbonate → HCID 67428163、化合物

HRID 1662628
ノート
印刷プレビュー

反応式

HRID 1662628 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 11430Potassium CarbonateHCID 887471-(2-Pyrimidinyl)piperazineHCID 27960291-Hydroxybenzotriazole hydrateHCID 21925457HCID 21925457、化合物HCID 22619321HCID 22619321、化合物

生成物 1

HCID 67428163HCID 67428163、化合物収率 94.6%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f059cd3530fd427d844483f5a1943187
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030499B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート