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

HRID 456422

反応式

HRID 456422 の反応式
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

参加物

7

反応条件

温度
160 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bfd189a0842d47fd8b77df7eb5d727b1
出典データセット
uspto-grants-2007_03
特許番号
US07186721B2

関連ノート

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