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Hydrochloric Acid → 4-Azatricyclo[4.3.1.13,8]undecane

HRID 2083582
ノート
印刷プレビュー

反応式

HRID 2083582 の反応式
C1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:9]=[N:10]C=C[CH:13]=2)C=CC=CC=1.C([Li])CCC.ClCCN1CC2CC3CC(CC1C3)C2.Cl>C1CCCCC1>[CH:14]12[CH2:7][CH:8]3[CH2:13][CH:16]([CH2:17][CH:18]([NH:10][CH2:9]3)[CH2:19]1)[CH2:15]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 772513-BenzhydrylpyridineHCID 539394214-(2-Chloroethyl)-4-azatricyclo[4.3.1.13,8]undecaneHCID 178418339Butyllithium

生成物 1

HCID 322724-Azatricyclo[4.3.1.13,8]undecane

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

Reaction of 2.5 parts of diphenyl-3-pyridylmethane in 60 parts by volume of cyclohexane with an equivalent amount of butyl lithium at 10° C under nitrogen is followed by the addition of 2.1 parts of 4-(2-chloroethyl)-4-azatricyclo[4.3.1.13,8 ]undecane [preparable by mixing the hydrochloride thereof (U.S. Pat. No. 3,845,038) with excess aqueous sodium carbonate, extracting the mixture with toluene, and consecutively washing the extract with water, drying it over anhydrous sodium sulfate, filtering out the drying agent, and removing the solvent by vacuum distillation]. Quenching of the reaction with water and isolation by extraction with ether, washing, drying and evaporation of solvent provides 4-[3,3-(diphenyl)-3-(3-pyridyl)propyl[-4-azatricyclo[4.3.1.13,8 ]undecane having the following structural formula ##STR52##

後処理

  1. extraction3,845,038) with excess aqueous sodium carbonate, extracting the mixture with toluene
  2. washconsecutively washing the
  3. extractionextract with water
  4. dry with materialdrying it over anhydrous sodium sulfate
  5. filtrationfiltering out the drying agent
  6. customremoving the solvent
  7. distillationby vacuum distillation]
  8. customQuenching of the reaction with water and isolation by extraction with ether
  9. washwashing
  10. customdrying
  11. customevaporation of solvent

出典と根拠

ORDレコード
ord-f1e7008cd2014a1f8404e94f2d073f00
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04086227

反応ノート

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