Water → HCID 11670326, 화합물

HRID 1713027노트

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HRID 1713027 반응식
C[O:2][C:3](=[O:34])[CH2:4][N:5]([C:7](=[O:33])[CH2:8][C:9]([CH3:32])([CH3:31])[CH2:10][N:11]1[C:28](=[S:29])[N:14]2[C:15]3[CH:16]=[C:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=4)[O:18][C:19]=3[CH:20]=[C:13]2[C:12]1=[O:30])[CH3:6].O.C(Cl)(Cl)Cl.C([O-])(O)=O.[Na+]>C(O)(C(F)(F)F)=O.CO>[Cl:27][C:24]1[CH:25]=[CH:26][C:21]([C:17]2[O:18][C:19]3[CH:20]=[C:13]4[C:12](=[O:30])[N:11]([CH2:10][C:9]([CH3:31])([CH3:32])[CH2:8][C:7]([N:5]([CH2:4][C:3]([OH:34])=[O:2])[CH3:6])=[O:33])[C:28](=[S:29])[N:14]4[C:15]=3[CH:16]=2)=[CH:22][CH:23]=1

참가 물질

7

반응물 4

HCID 962Water2회HCID 6212ChloroformHCID 516892Sodium BicarbonateHCID 11497027HCID 11497027, 화합물

생성물 1

HCID 11670326HCID 11670326, 화합물수율 88%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6422Trifluoroacetic acid용매

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온도
40 °C

실험 절차

Compound 20 was dissolved in TFA (1.5 ml) and water (0.75 ml) was added thereto. The resulting mixture was stirred at 40° C. for 16 hours. After cooling the mixture to room temperature, water and chloroform were added, followed by addition of 10% NaHCO3 (20 ml), while maintaining an acidic pH of the solution. The organic layer was separated, washed twice with water, dried over Na2SO4 and the solvent was evaporated under reduced pressure to give an orange solid. Chromatography purification was carried out using with a 8:2 ethyl acetate:methanol mixture as eluent to give Compound 21 (38.3 mg, 88% yield) as a yellow solid.

후처리

  1. temperatureAfter cooling the mixture to room temperature
  2. temperaturewhile maintaining an acidic pH of the solution
  3. customThe organic layer was separated
  4. washwashed twice with water
  5. dry with materialdried over Na2SO4
  6. customthe solvent was evaporated under reduced pressure
  7. customto give an orange solid
  8. customChromatography purification

출처 및 근거

ORD 기록
ord-8eae679ba8e841b2903be103be0951a2
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795255B2

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