Water → N-(4-Fluorophenyl)-N'-(4-{[2-(2-oxotetrahydro-1H-1-pyrrolyl)-4-pyridyl]oxy}phenyl)urea

HRID 1433469노트

반응식

HRID 1433469 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]3[CH:24]=[CH:23][N:22]=[C:21]([NH:25][C:26](=[O:31])[CH2:27][CH2:28][CH2:29]Cl)[CH:20]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.O>C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]3[CH:24]=[CH:23][N:22]=[C:21]([N:25]4[CH2:29][CH2:28][CH2:27][C:26]4=[O:31])[CH:20]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 22936908N-(4-Fluorophenyl)-N'-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea

생성물 1

HCID 22936528N-(4-Fluorophenyl)-N'-(4-{[2-(2-oxotetrahydro-1H-1-pyrrolyl)-4-pyridyl]oxy}phenyl)urea수율 40.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

N-(4-Fluorophenyl)-N′-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea (56 mg), potassium carbonate (46 mg) and dimethylformamide (2 ml) were stirred at 150° C. for 15 minutes. Water and ethyl acetate were added for extraction, and the extract was passed through a glass filter coated with silica gel. The silica gel was washed with ethyl acetate, and the organic layer was distilled off under reduced pressure. Ethyl acetate and hexane were added to the residue, and the precipitated solid was filtered out to obtain 21 mg of a faint brown powder.

후처리

  1. filtrationfilter
  2. washThe silica gel was washed with ethyl acetate
  3. distillationthe organic layer was distilled off under reduced pressure
  4. additionEthyl acetate and hexane were added to the residue
  5. filtrationthe precipitated solid was filtered out

출처 및 근거

ORD 기록
ord-06598e9eac6644f8b5cf5715812f4891
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612092B2

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