Methanol → HCID 178428390、化合物

HRID 80210

反応式

HRID 80210 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178428390HCID 178428390、化合物収率 31.97%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0750910891304fd081d297fb9e627de7
出典データセット
uspto-grants-2014_09
特許番号
USRE045173E1

関連ノート

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