Citric Acid → HCID 15745308、化合物

HRID 373579

反応式

HRID 373579 の反応式
[CH2:1]([N:5]1[CH2:12][CH:11]2[C:13]([CH3:15])([CH3:14])[CH:7]([CH2:8][NH:9][CH2:10]2)[CH2:6]1)[CH2:2][CH2:3][CH3:4].[NH2-].[Li+].[CH3:18][C:19]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][C:20]=1[CH2:21]Cl.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CN(C)C=O>[CH2:1]([N:5]1[CH2:6][CH:7]2[C:13]([CH3:14])([CH3:15])[CH:11]([CH2:10][N:9]([CH2:21][C:20]3[CH:23]=[C:24]([CH3:27])[CH:25]=[CH:26][C:19]=3[CH3:18])[CH2:8]2)[CH2:12]1)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 311Citric Acid2 回HCID 24532Lithium amideHCID 69987Benzene, 2-(chloromethyl)-1,4-dimethyl-HCID 14369008HCID 14369008、化合物

生成物 1

HCID 15745308HCID 15745308、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
60 °C

実験手順

3.5 g 3-n-butyl-9,9-dimethyl-3, 7-diazabicyclo[3,3,1]nonane were dissolved in 25 ml of dimethyl formamide, and 0.8 g of lithium amide was added to the solution. The reaction mixture was then maintained at a temperature of 60° C. for 1 hour and subsequently allowed to cool. After cooling, a solution of 5.6 g of 2,5-dimethylbenzyl chloride in 10 ml of dimethyl formamide was added dropwise, and the reaction mixture was stirred for a further 4 hours at 80° C. Then aqueous citric acid solution was added to the reaction mixture in order to dissolve the title compound as a citric acid salt. The solution was washed with diethyl ether and then rendered alkaline by adding dilute sodium hydroxide solution, whereupon the title compound was again freed as a base. The free base was extracted with diethyl ether. After the ether extract was dried over magnesium sulfate, the ether solution was filtered, and the ether was distilled off. The remaining oil was purified by distillation in a bulb tube at 210° C. and 0.01 Torr.

後処理

  1. temperatureto cool
  2. temperatureAfter cooling

出典と根拠

ORDレコード
ord-8ff9bd8605bb45d18e2451b432d0c145
出典データセット
uspto-grants-1992_11
特許番号
US05164401

関連ノート

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