Chlorotrimethylsilane → Ondansetron

HRID 2112268

반응식

HRID 2112268 반응식
CN1[CH2:7][N:6]([CH3:8])[CH2:5][N:4]([CH3:9])C1.Cl[Si](C)(C)C.[CH3:15][N:16]1[C:28]2[CH2:27][CH2:26][CH2:25][C:24](=[O:29])[C:23]=2[C:22]2[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=2.[CH3:30]C1NC=CN=1>C(#N)C.C1(C)C=CC=CC=1>[CH3:15][N:16]1[C:28]2[CH2:27][CH2:26][CH:25]([CH2:8][N:6]3[CH:7]=[CH:9][N:4]=[C:5]3[CH3:30])[C:24](=[O:29])[C:23]=2[C:22]2[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=2

참가 물질

7

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 79521,3,5-Trimethyl-1,3,5-triazacyclohexaneHCID 127492-MethylimidazoleHCID 5988759-Methyl-1,2,3,9-tetrahydro-4H-carbazol-4-one

생성물 1

HCID 4595Ondansetron수율 54%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6342Acetonitrile용매

실험 절차

To the solution 19.5 g of 1,3,5-trimethylhexahydro-1,3,5-triazine in 20 ml of actonitrile and 150 ml of toluene, was slowly added 19 ml of chlorotrimethylsilane, which was then stirred for 10 min. 10 g of 1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one and 8.2 g of 2-methyl imidazole was subsequently added to the reaction mixture, which was then stirred under reflux. After completion of reaction, the reaction mixture was evaporated, and then 200 ml of water was added to the resulting residue, which was then stirred for 2 hours at room temperature. The resulting solid was filtered and washed with water to give 7.95 g of light yellow title compound (yield 54%).

후처리

  1. stirringwas then stirred
  2. temperatureunder reflux
  3. customAfter completion of reaction
  4. customthe reaction mixture was evaporated
  5. addition200 ml of water was added to the resulting residue, which
  6. stirringwas then stirred for 2 hours at room temperature
  7. filtrationThe resulting solid was filtered
  8. washwashed with water

출처 및 근거

ORD 기록
ord-df8577f54fd841fe8d572290c581f89a
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521565B2

연결된 노트

불러오는 중…