Hydrochloric Acid → HCID 67059991, 화합물

HRID 238282노트

반응식

HRID 238282 반응식
N[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:16])[CH3:15])[CH2:10][CH2:9]1.N([O-])=O.[Na+].[ClH:21]>O.[Cu]Cl>[Cl:21][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:16])[CH3:15])[CH2:10][CH2:9]1

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 23668193Sodium NitriteHCID 67059966HCID 67059966, 화합물

생성물 1

HCID 67059991HCID 67059991, 화합물

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

1-[4-(2-Amino-phenyl)-piperidin-1-yl]-ethanone (0.3 g, 1.38 mmol) was dissolved in a solution of hydrochloric acid (6 N, 6 mL) and cooled to 0° C. A solution of sodium nitrite (0.097 g, 1.4 mmol) in water (1 mL) was added drop wise and the mixture stirred for 1 hour. The resulting solution was added drop wise to a solution of copper (I) chloride (0.35 g, 3.5 mmol) in hydrochloric acid (6 N, 6 mL). The mixture was allowed to warm to room temperature, and was then diluted with water (20 mL) and the products extracted into ethyl acetate. The organic solution was washed with water (20 mL) then dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum to give the title compound as an orange oil (0.2 g). LCMS m/z 238.2 [M+H]+. R.T.=4.30 min (Analytical Method 4).

후처리

  1. temperatureto warm to room temperature
  2. extractionthe products extracted into ethyl acetate
  3. washThe organic solution was washed with water (20 mL)
  4. dry with materialthen dried over magnesium sulphate
  5. filtrationfiltered
  6. customthe solvent removed by evaporation under vacuum

출처 및 근거

ORD 기록
ord-eb082fa7e0374f369463be11d1a9735c
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642621B2

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