Dichloromethane → HCID 68585192、化合物

HRID 17476

反応式

HRID 17476 の反応式
C(N(C(C)C)CC)(C)C.[CH3:10][NH:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1.ClCCl.Cl[C:22]1[O:23][C:24]2[C:25](=[C:27]([C:39]#[N:40])[C:28]([CH3:38])=[C:29]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[C:30]=2[F:31])[N:26]=1>C(OCC)(=O)C>[F:31][C:30]1[C:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[C:28]([CH3:38])[C:27]([C:39]#[N:40])=[C:25]2[C:24]=1[O:23][C:22]([N:11]([CH3:10])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1)=[N:26]2

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 207272-Pyridinamine, N-methyl-HCID 81531DiisopropylethylamineHCID 510414292-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

生成物 1

HCID 68585192HCID 68585192、化合物収率 57.7%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

Diisopropylethylamine (169 μl, 0.944 mmol) and 2-(methylamino)pyridine (102 μl, 0.994 mmol) were added to a dichloromethane (10 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (190 mg, 0.663 mmol), followed by heating under reflux in an oil bath at 50° C. for 3 hours. The reaction liquid was cooled to room, temperature, ethyl acetate (70 ml) was added, followed by washing with water (50 ml) and saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=4:1) to obtain the entitled compound (137 mg, 57.5%) as a colorless solid.

後処理

  1. temperatureby heating
  2. customThe reaction liquid
  3. additionwas added
  4. washby washing with water (50 ml) and saturated brine (50 ml)
  5. dry with materialAfter drying over anhydrous sodium sulfate and concentration under reduced pressure
  6. customthe resulting residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-f1b148179b7e4b379a627f9581f4c5fc
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

関連ノート

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