Morpholine → 2-Benzyl-2-(dimethylamino)-1-(4-(morpholin-4-yl)phenyl)butan-1-one

HRID 742509

反応式

HRID 742509 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:22])[C:9]([N:19]([CH3:21])[CH3:20])([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:10][CH3:11])=[CH:4][CH:3]=1.[NH:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1.C([O-])([O-])=O.[K+].[K+]>CS(C)=O>[CH2:12]([C:9]([N:19]([CH3:21])[CH3:20])([CH2:10][CH3:11])[C:8]([C:5]1[CH:6]=[CH:7][C:2]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[CH:3][CH:4]=1)=[O:22])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 193605992-Benzyl-2-(dimethylamino)-1-(4-fluorophenyl)butan-1-one

生成物 1

HCID 861712-Benzyl-2-(dimethylamino)-1-(4-(morpholin-4-yl)phenyl)butan-1-one

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

608.7 g (2.03 tool) of 1-(4-fluorophenyl)-2-dimethylamino-2-benzyl-butan-1-one (Example 1, B), 354.2 g (4.06 tool) of morpholine, 562 g (4.06 tool) of K2CO3 and 2000 ml of dimethylsulfoxide are heated at 160° for 12 hours, with stirring. After this time, a sample no longer shows any starting ketone in a thin-layer chromatogram. The reaction solution is cooled to room temperature, poured onto ice and extracted with methylene chloride. The organic phase is dried over MgSO4, filtered and evaporated. The oily residue crystallizes from ethanol. The product melts at 111°-119°.

後処理

  1. additionpoured onto ice
  2. extractionextracted with methylene chloride
  3. dry with materialThe organic phase is dried over MgSO4
  4. filtrationfiltered
  5. customevaporated
  6. customThe oily residue crystallizes from ethanol

出典と根拠

ORDレコード
ord-3035fb41dbb54ac2a802b831bc305fdc
出典データセット
uspto-grants-1996_09
特許番号
US05554663

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