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Acetyl chloride → N-[6-(8-acetyloctahydro-2H-pyrazino[1,2-a]pyrazin-2-yl)-4-(4-fluoro-2-methylphenyl)-3-pyridinyl]-2-[3,5-bis(trifluoromethyl)phenyl]-N,2-dimethylpropanamide

HRID 2074930
ノート
印刷プレビュー

反応式

HRID 2074930 の反応式
[F:1][C:2]([F:45])([F:44])[C:3]1[CH:4]=[C:5]([C:13]([CH3:43])([CH3:42])[C:14]([N:16]([C:18]2[CH:19]=[N:20][C:21]([N:32]3[CH2:37][CH2:36][N:35]4[CH2:38][CH2:39][NH:40][CH2:41][CH:34]4[CH2:33]3)=[CH:22][C:23]=2[C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=2[CH3:31])[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.C(N(CC)CC)C.[C:53](Cl)(=[O:55])[CH3:54]>ClCCl>[C:53]([N:40]1[CH2:39][CH2:38][N:35]2[CH2:36][CH2:37][N:32]([C:21]3[N:20]=[CH:19][C:18]([N:16]([CH3:17])[C:14](=[O:15])[C:13]([C:5]4[CH:4]=[C:3]([C:2]([F:44])([F:1])[F:45])[CH:8]=[C:7]([C:9]([F:11])([F:10])[F:12])[CH:6]=4)([CH3:43])[CH3:42])=[C:23]([C:24]4[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=4[CH3:31])[CH:22]=3)[CH2:33][CH:34]2[CH2:41]1)(=[O:55])[CH3:54]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 592157712-[3,5-bis(trifluoromethyl)phenyl]-N-[4-(4-fluoro-2-methyl phenyl)-6-(octahydro-2H-pyrazino[1,2-a]pyrazin-2-yl)-3-pyridinyl]-N,2-dimethylpropanamide

生成物 1

HCID 15983979N-[6-(8-acetyloctahydro-2H-pyrazino[1,2-a]pyrazin-2-yl)-4-(4-fluoro-2-methylphenyl)-3-pyridinyl]-2-[3,5-bis(trifluoromethyl)phenyl]-N,2-dimethylpropanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of crude 2-[3,5-bis(trifluoromethyl)phenyl]-N-[4-(4-fluoro-2-methyl phenyl)-6-(octahydro-2H-pyrazino[1,2-a]pyrazin-2-yl)-3-pyridinyl]-N,2-dimethylpropanamide (prepared with an analogous procedure to that described for D80, 89 mg, 0.14 mmol) in 5 mL of dichloromethane were added at 0° C. triethylamine (197 μL, 1.41 mmol) and acetyl chloride (75 μL, 1.0 mmol). The reaction was left at room temperature for 2 h. It was diluted with dichloromethane, extracted with sat NaHCO3 solution, the organics dried (Na2SO4), and the solvent was removed. The product was purified by flash chromatography (silica, cyclohexane:EtOAc 50:50 to EtOAc). Obtained 60 mg.

後処理

  1. extractionextracted with sat NaHCO3 solution
  2. dry with materialthe organics dried (Na2SO4)
  3. customthe solvent was removed
  4. customThe product was purified by flash chromatography (silica, cyclohexane:EtOAc 50:50 to EtOAc)
  5. customObtained 60 mg

出典と根拠

ORDレコード
ord-4d2cb29a0ba645d498a2f47da765367a
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919491B2

反応ノート

読み込み中…

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