Methanol → HCID 178428390, 화합물

HRID 80210

반응식

HRID 80210 반응식
[CH:1]1([C:4]([C:6]2[CH:11]=[CH:10][C:9]([N:12]3[CH2:16][CH2:15][N:14]([C:17]4[CH:18]=[N:19][CH:20]=[CH:21][C:22]=4[CH3:23])[C:13]3=[O:24])=[CH:8][C:7]=2F)=O)[CH2:3][CH2:2]1.CO.O.[NH2:29][NH2:30]>C(Cl)(Cl)Cl>[CH:1]1([C:4]2[C:6]3[C:7](=[CH:8][C:9]([N:12]4[CH2:16][CH2:15][N:14]([C:17]5[CH:18]=[N:19][CH:20]=[CH:21][C:22]=5[CH3:23])[C:13]4=[O:24])=[CH:10][CH:11]=3)[NH:30][N:29]=2)[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 596361401-(4-Cyclopropanecarbonyl-3-fluoro-phenyl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

생성물 1

HCID 178428390HCID 178428390, 화합물수율 31.97%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
120 °C

실험 절차

1-(4-Cyclopropanecarbonyl-3-fluoro-phenyl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (I-161b: 175 mg, 0.516 mmol) in hydrazine hydrate solution (10 mL) was taken in a reaction flask. The flask was refluxed at 120° C. overnight. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was cooled to room temperature and partitioned between ice water and chloroform. The organic layer was dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (4% MeOH in CHCl3), followed by hexane and ether wash, afforded 55 mg of the product (31.97% yield).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. custompartitioned between ice water and chloroform
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by column chromatography on silica gel (4% MeOH in CHCl3)
  6. washwash

출처 및 근거

ORD 기록
ord-0750910891304fd081d297fb9e627de7
출처 데이터셋
uspto-grants-2014_09
특허 번호
USRE045173E1

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