Sodium Iodide → 4-(Morpholin-4-yl)benzamide

HRID 56114

反応式

HRID 56114 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=1.[Na+].[I-].C([O-])([O-])=O.[K+].[K+].[CH2:19]([O:22][CH2:23][CH2:24]Cl)[CH2:20]Cl>CN(C=O)C.O>[O:22]1[CH2:23][CH2:24][N:1]([C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=2)[CH2:20][CH2:19]1

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 8115Bis(2-chloroethyl) etherHCID 11430Potassium CarbonateHCID 760794-Aminobenzamide

生成物 1

HCID 221422424-(Morpholin-4-yl)benzamide収率 64%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

To a solution of 4-aminobenzamide (6.81 g, 50 mmol) in DMF (70 mL) were added NaI (22.48 g, 150 mmol) and K2CO3 (13.82 g, 100 mmol). The mixture was heated to 140° C. and 2,2′-dichlorodiethyl ether (14.30 g, 100 mmol) was added. The reaction mixture was heated at 150° C. for 5 h, and cooled to rt. The mixture was diluted with water (100 mL), stirred for 10 min, and filtered. The filter cake was washed with water and dried to give the title compound as a yellow solid (6.60 g, 64%).

後処理

  1. temperatureThe reaction mixture was heated at 150° C. for 5 h
  2. temperaturecooled to rt
  3. filtrationfiltered
  4. washThe filter cake was washed with water
  5. customdried

出典と根拠

ORDレコード
ord-c5a4edc26e8649629981307c9899858c
出典データセット
uspto-grants-2016_09
特許番号
US09434695B2

関連ノート

読み込み中…