Chlorotrimethylsilane → Ondansetron

HRID 2112268

反応式

HRID 2112268 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 4595Ondansetron収率 54%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-df8577f54fd841fe8d572290c581f89a
出典データセット
uspto-grants-2009_04
特許番号
US07521565B2

関連ノート

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