Water → Olanzapine

HRID 1666935노트

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HRID 1666935 반응식
[NH2:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[NH:4][C:5]1[S:6][C:7]([CH3:12])=[CH:8][C:9]=1[C:10]#[N:11].ClCCl.O.[CH3:21][N:22]1[CH2:27][CH2:26]N[CH2:24][CH2:23]1>Cl.CN1CCNCC1>[CH3:12][C:7]1[S:6][C:5]2[NH:4][C:3]3[CH:13]=[CH:14][CH:15]=[CH:16][C:2]=3[N:1]=[C:10]([N:11]3[CH2:26][CH2:27][N:22]([CH3:21])[CH2:23][CH2:24]3)[C:9]=2[CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 531671-MethylpiperazineHCID 674452622-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile

생성물 1

HCID 135398745Olanzapine

시약·촉매·용매 1

HCID 121968951-Methylpiperazine hydrochloride용매

반응 조건

온도
120 °C

실험 절차

2-(2-Aminoanilino)-5-methylthiophene-3-carbonitrile (10.0 g) is taken in N-methyl-piperazine (60 ml) and N-methyl-piperazine hydrochloride (24 gm). The solution is heated at 120° C. until completion of reaction. The reaction mass is cooled and dichloromethane (100 ml) and water is added. The mixture is cooled up to room temperature and dichloromethane layer is separated. 50 ml dichloromethane is evaporated and cyclohexane is added in clear solution. On Cooling the solution, solid is separated out, which is filtered and dried under vacuum to get Olanzapine Form I. (Purity >99.6%)

후처리

  1. temperatureThe reaction mass is cooled
  2. temperatureThe mixture is cooled up to room temperature
  3. customdichloromethane layer is separated
  4. custom50 ml dichloromethane is evaporated
  5. additioncyclohexane is added in clear solution
  6. temperatureOn Cooling the solution, solid
  7. customis separated out
  8. filtrationwhich is filtered
  9. customdried under vacuum

출처 및 근거

ORD 기록
ord-8deccf48941d4bf2a5acbabb0be7147a
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044196B2

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