Hydrochloric Acid → HCID 67059991、化合物

HRID 238282ノート

反応式

HRID 238282 の反応式
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

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 23668193Sodium NitriteHCID 67059966HCID 67059966、化合物

生成物 1

HCID 67059991HCID 67059991、化合物

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eb082fa7e0374f369463be11d1a9735c
出典データセット
uspto-grants-2014_02
特許番号
US08642621B2

反応ノート

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