Dichloromethane → HCID 68585192, 화합물

HRID 17476

반응식

HRID 17476 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 68585192HCID 68585192, 화합물수율 57.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-f1b148179b7e4b379a627f9581f4c5fc
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

연결된 노트

불러오는 중…