Water → HCID 19434874, 화합물

HRID 1736216노트

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HRID 1736216 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[C:18]([F:19])=[CH:17][C:16]([F:20])=[C:15]([NH:21][CH2:22][CH2:23][CH:24]=[C:25]([CH3:27])[CH3:26])[C:11]=3[C:12](=[O:14])[CH:13]=2)=[CH:4][C:3]=1[F:28].S(=O)(=O)(O)[OH:30].O>C(O)C>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[C:18]([F:19])=[CH:17][C:16]([F:20])=[C:15]([NH:21][CH2:22][CH2:23][CH2:24][C:25]([OH:30])([CH3:26])[CH3:27])[C:11]=3[C:12](=[O:14])[CH:13]=2)=[CH:4][C:3]=1[F:28]

참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 194349092-(4-Amino-3-fluorophenyl)-6,8-difluoro-5-(4-methyl-3-pentenylamino)-4H-1-benzopyran-4-one

생성물 1

HCID 19434874HCID 19434874, 화합물수율 84%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

16 mg (0.041 mmol) of Compound 137 obtained in Example 137 was dissolved in 3 mL of ethanol, 3 mL of 50% sulfuric acid was added and the mixture was stirred at 100° C. for 1 hour. The reaction solution was cooled on ice, water was added and the mixture was extracted twice with ethyl acetate. The organic layer was washed once with an aqueous saturated solution of sodium bicarbonate, once with water and once with an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 14 mg of Compound 138 (yield: 84%).

후처리

  1. additionwas added
  2. extractionthe mixture was extracted twice with ethyl acetate
  3. washThe organic layer was washed once with an aqueous saturated solution of sodium bicarbonate, once with water and once with an aqueous saturated solution of sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-8b8cf33894cc4250b27616f1d3433195
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05539112

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