Water → 3-(4-(4-Methylpiperazin-1-yl)phenyl)butanamide

HRID 1896282ノート

反応式

HRID 1896282 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]#[N:17])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[OH2:19]>C(=O)(O)[O-].[Na+]>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]([NH2:17])=[O:19])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1

参加物

4

反応物 2

HCID 962WaterHCID 673833103-(4-(4-Methylpiperazin-1-yl)phenyl)butanenitrile

生成物 1

HCID 673827633-(4-(4-Methylpiperazin-1-yl)phenyl)butanamide収率 74%

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
90 °C

実験手順

A suspension of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanenitrile (450 mg, 1.85 mmol) and poly phosphoric acid (4.5 g) was heated at 90° C. for 3 h. The reaction mixture was cooled to room temperature, diluted with cold water and basified with saturated sodium bicarbonate solution. The aqueous layer was extracted with DCM, washed with water and brine solution. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to afford 360 mg (74%) of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanamide as light yellow color solid.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe aqueous layer was extracted with DCM
  3. washwashed with water and brine solution
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8a4e5ab7cc10455bad64765bfc3a8286
出典データセット
uspto-grants-2013_08
特許番号
US08518948B2

反応ノート

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