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

HRID 742509

반응식

HRID 742509 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-3035fb41dbb54ac2a802b831bc305fdc
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554663

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