Sodium Hydroxide → N,N'-diheptyl-p-xylylenediamine

HRID 1770049ノート

反応式

HRID 1770049 の反応式
[CH2:1]([NH:8][C:9](=O)[C:10]1[CH:25]=[CH:24][C:13]([C:14]([NH:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=O)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[H-].COCCO[Al+]OCCOC.[OH-].[Na+]>C1(C)C=CC=CC=1>[CH2:17]([NH:16][CH2:14][C:13]1[CH:12]=[CH:11][C:10]([CH2:9][NH:8][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[CH:25][CH:24]=1)[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 4098298N,N'-diheptylterephthalamideHCID 22591236HCID 22591236、化合物

生成物 1

HCID 14801556N,N'-diheptyl-p-xylylenediamine収率 97.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a mixture of 3.6 g N,N'-diheptylterephthalamide obtained in Example 1 and 60 ml toluene, was added dropwise 15.6 ml of a 70% solution of bis(2-methoxyethoxy)aluminum hydride in toluene. After heating under reflux for three hours, the reaction mixture was treated with 30 ml of 2.5N aqueous caustic soda solution under ice cooling, and the toluene layer separated was washed with saturated aqueous solution of sodium chloride and dried over a drying agent. Distilling off the solvent from the dried solution gave 3.24 g of N,N'-diheptyl-p-xylylenediamine.

後処理

  1. temperatureAfter heating
  2. temperatureunder reflux for three hours
  3. customthe toluene layer separated
  4. washwas washed with saturated aqueous solution of sodium chloride
  5. customdried over a drying agent
  6. distillationDistilling off the solvent from the dried solution

出典と根拠

ORDレコード
ord-b59ae24b340c4160b73bb2f15813942f
出典データセット
uspto-grants-1995_01
特許番号
US05384425

反応ノート

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