Water → N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine

HRID 37295

反応式

HRID 37295 の反応式
[C:1]1([CH:7]2[CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:14]1([CH2:20][NH2:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.O>C1C=CC=CC=1>[C:1]1([CH:7]2[CH2:12][CH2:11][CH:10]([NH:21][CH2:20][CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 76688CyclohexanemethylamineHCID 786054-Phenylcyclohexanone

生成物 1

HCID 19935094N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 5 g of 4-phenylcyclohexanone and cyclohexylmethylamine in 100 ml of benzene was refluxed for 2 hours with removing water and the solvent was distilled away in vacuo. The residue was dissolved in methanol and to the solution was added 1.5 g of sodium borohydride. The mixture was stirred at room temperature and the solvent was distilled away in vacuo. To the residue was added water and extracted with diethyl ether. The organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was distilled away to give 7 g of N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine as an oil. (N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine hydrochloride, melting at 267°-270° C. with decomposition)

後処理

  1. distillationthe solvent was distilled away in vacuo
  2. dissolutionThe residue was dissolved in methanol and to the solution
  3. additionwas added 1.5 g of sodium borohydride
  4. distillationthe solvent was distilled away in vacuo
  5. additionTo the residue was added water
  6. extractionextracted with diethyl ether
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over magnesium sulfate
  9. distillationThe solvent was distilled away

出典と根拠

ORDレコード
ord-8915cbe5c8664ef18622aa95456bc4f5
出典データセット
uspto-grants-1995_05
特許番号
US05420164

関連ノート

読み込み中…