Water → HCID 23156433, 화합물

HRID 228535

반응식

HRID 228535 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[N:12]=[CH:11][CH:10]=2)=[CH:4][C:3]=1[CH2:23][OH:24].Cl[C:26](Cl)([O:28]C(=O)OC(Cl)(Cl)Cl)Cl.O>C(N(CC)CC)C.C1(C)C=CC=CC=1>[CH3:20][O:19][C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][C:15]=1[O:21][CH3:22])[N:12]=[CH:11][CH:10]=[C:9]2[O:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:26](=[O:28])[O:24][CH2:23][C:3]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 94429TriphosgeneHCID 68830546HCID 68830546, 화합물

생성물 1

HCID 23156433HCID 23156433, 화합물수율 39%

시약·촉매·용매 1

HCID 22504574Toluene triethylamine용매

실험 절차

{2-Amino-5-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}methanol (63 mg) was dissolved in heated triethylamine/toluene (1.2 ml/6 ml) to prepare a solution. Triphosgene (98 mg) was added to the solution and was heated under reflux for 2 min. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with chloroform. The chloroform layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography on silica gel using acetone-chloroform to give the title compound (24 mg, yield 39%).

후처리

  1. customto prepare a solution
  2. temperaturewas heated
  3. temperatureunder reflux for 2 min
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was then washed with water and saturated brine
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. customThe solvent was removed
  8. distillationby distillation under the reduced pressure
  9. customthe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-f33e7705410f4bfdb218846039397b48
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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