Hydrochloric Acid → HCID 178436219, 화합물

HRID 1455749노트

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HRID 1455749 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[C:11]1[N:16]=[C:15]([O:17]C)[C:14]([CH2:19][N:20]([CH3:31])[C@@H:21]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:24][CH2:23][CH2:22]2)=[C:13]([CH3:32])[N:12]=1)[CH3:2].CCO.Cl.[OH-].[Na+]>CCOC(C)=O>[CH2:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([CH2:1][CH3:2])[C:4]=1[C:11]1[N:16]=[C:15]([OH:17])[C:14]([CH2:19][N:20]([CH3:31])[C@@H:21]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:24][CH2:23][CH2:22]2)=[C:13]([CH3:32])[N:12]=1)[CH3:10]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 57531359(1S)-N-{[2-(2,6-diethylphenyl)-4-methoxy-6-methylpyrimidin-5-yl]methyl}-N-methyl-1,2,3,4-tetrahydronaphthalen-1-amine

생성물 1

HCID 178436219HCID 178436219, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

To a flask containing (1S)-N-{[2-(2,6-diethylphenyl)-4-methoxy-6-methylpyrimidin-5-yl]methyl}-N-methyl-1,2,3,4-tetrahydronaphthalen-1-amine (3.5 g, 8.15 mmol) is added EtOH (50 mL) and HCl (12 N, 50 mL) and the solution is heated at 90° C. for 16 h. The solution is cooled to 0° C. and basified using 5N NaOH slowly, followed by addition of EtOAc (100 mL). The organic layer is washed with sat. NaHCO3 (100 mL), brine (100 mL) and dried over Na2SO4. Concentration and vacuum drying affords the title compound as a white gummy foam. [mass expected (415.57); mass found (415.33)]

후처리

  1. temperatureThe solution is cooled to 0° C.
  2. washThe organic layer is washed with sat. NaHCO3 (100 mL), brine (100 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationConcentration and vacuum
  5. customdrying

출처 및 근거

ORD 기록
ord-2a8ab1d34bc743d0aeb8e2074aa25642
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07482350B2

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