Diisopropylethylamine → (R)-2-[6-(4-Trifluoromethyl-phenyl)-pyridazin-3-yl]-octahydro-pyrido[1,2-a]pyrazine

HRID 456422

반응식

HRID 456422 반응식
C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.[CH2:15]1[NH:20][CH2:19][CH2:18][N:17]2[CH2:21][CH2:22][CH2:23][CH2:24][C@H:16]12.C(N(C(C)C)CC)(C)C.Cl[C:35]1[N:36]=[N:37][C:38]([C:41]2[CH:46]=[CH:45][C:44]([C:47]([F:50])([F:49])[F:48])=[CH:43][CH:42]=2)=[CH:39][CH:40]=1>ClCCl.CS(C)=O>[F:50][C:47]([F:48])([F:49])[C:44]1[CH:43]=[CH:42][C:41]([C:38]2[N:37]=[N:36][C:35]([N:20]3[CH2:19][CH2:18][N:17]4[CH2:21][CH2:22][CH2:23][CH2:24][C@@H:16]4[CH2:15]3)=[CH:40][CH:39]=2)=[CH:46][CH:45]=1

참가 물질

7

반응 조건

온도
160 °C

실험 절차

A mixture of the dihydrochloride salt of (R)-octahydropyrido[1,2-a]pyrazine (649 mg, 3.05 mmol), diisopropylethylamine (1.17 ml, 6.72 mmol), 3-chloro-6-(4-trifluoromethylphenyl)-pyridazine (290 mg, 1.12 mmol) and dimethylsulfoxide (1 ml) was heated in a closed vessel at 160° C. for 40 min. The reaction mixture was cooled to room temperature, diluted with dichloromethane (10 ml) and washed with water (2×15 ml) and brine (15 ml). The organic layer was dried over magnesium sulphate. The solvent was removed in vacuo to give 398 mg of the title compound as the free base.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washwashed with water (2×15 ml) and brine (15 ml)
  3. dry with materialThe organic layer was dried over magnesium sulphate
  4. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-bfd189a0842d47fd8b77df7eb5d727b1
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186721B2

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