Hydrochloric Acid → HCID 178436219, 화합물

HRID 1091929노트

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HRID 1091929 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-3ea80cc2e6044f829770278ebeff30c5
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129395B2

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