Triethylamine → 3-ethoxy-4-{[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl)amino}-3-cyclobutene-1,2-dione

HRID 459656노트

반응식

HRID 459656 반응식
[CH3:1][N:2]1[C:6]([NH:7][C:8]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:5]([NH2:27])[CH:4]=[N:3]1.C(N(CC)CC)C.[CH3:35][CH2:36][O:37][C:38]1[C:42](=O)[C:40](=[O:41])[C:39]=1[O:44]CC.C(OCC)(=O)C>C(O)C.CCCCCC>[CH2:36]([O:37][C:38]1[C:39](=[O:44])[C:40](=[O:41])[C:42]=1[NH:27][C:5]1[CH:4]=[N:3][N:2]([CH3:1])[C:6]=1[NH:7][C:8]([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH3:35]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 123228Diethyl squarateHCID 685167251-methyl-N5-trityl-1H-pyrazole-4,5-diamine

생성물 1

HCID 219045093-ethoxy-4-{[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl)amino}-3-cyclobutene-1,2-dione

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8058Hexane용매

실험 절차

To a suspension of 1-methyl-N5-trityl-1H-pyrazole-4,5-diamine 1.60 g) in ethanol (50 ml) were added triethylamine (0.627 ml) and diethyl squarate (0.858 ml), and the mixture was stirred at room temperature for 22 hours. To the reaction mixture were added ethyl acetate (200 ml) and hexane (100 ml), and the solution was washed successively with water, 5% aqueous citric acid solution and brine. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crystalline residue was washed with diethyl ether and dried in vacuo to give 3-ethoxy-4-{[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino}-3-cyclobutene-1,2-dione (1.45 g) as a solid.

후처리

  1. washthe solution was washed successively with water, 5% aqueous citric acid solution and brine
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. washThe crystalline residue was washed with diethyl ether
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-b2a04be7d9da44ce801bfd7ee17385cb
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192943B2

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