Sodium Chloride → HCID 86593418, 화합물

HRID 1247846노트

반응식

HRID 1247846 반응식
S(O)(O)(=O)=O.[F:6][CH2:7][CH2:8][N:9]1[C:13]([NH2:14])=[C:12]([NH2:15])[CH:11]=[N:10]1.O=C1CCC(=O)N1[O:23][C:24](=O)[CH2:25][CH2:26][NH:27][C:28](=[O:34])[O:29][C:30]([CH3:33])([CH3:32])[CH3:31].C(=O)([O-])O.[Na+].[Cl-].[Na+]>O1CCCC1>[NH2:14][C:13]1[N:9]([CH2:8][CH2:7][F:6])[N:10]=[CH:11][C:12]=1[NH:15][C:24](=[O:23])[CH2:25][CH2:26][NH:27][C:28](=[O:34])[O:29][C:30]([CH3:31])([CH3:32])[CH3:33]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 516892Sodium BicarbonateHCID 10684599Boc-Beta-Ala-OSuHCID 69462687HCID 69462687, 화합물

생성물 1

HCID 86593418HCID 86593418, 화합물수율 58.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 1-(2-fluoroethyl)-1H-pyrazole-4,5-diamine sulfate (3 g) in tetrahydrofuran (30 ml) were added tert-butyl {3-[(2,5-dioxo-1-pyrrolidinyl)oxy]-3-oxopropyl}carbamate (3.9 g) and N,N-diisoporpylethylamine (3.5 g) under ice-cooling. The reaction mixture was stirred at room temperature for 2 hours. An aqueous sodium hydrogen carbonate solution and sodium chloride were added, and the mixture was extracted with ethyl acetate-tetrahydrofuran (three times). The organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel (ethyl acetate→ethyl acetate:ethanol=8:1) to give tert-butyl (3-{[5-amino-1-(2-fluoroethyl)-1H-pyrazol-4-yl]amino}-3-oxopropyl)carbamate (2.3 g).

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate-tetrahydrofuran (three times)
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel (ethyl acetate→ethyl acetate:ethanol=8:1)

출처 및 근거

ORD 기록
ord-096a1cd3f0504a95be7ba41c1050b414
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129232B2

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