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

HRID 2083582
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HRID 2083582 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 322724-Azatricyclo[4.3.1.13,8]undecane

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-f1e7008cd2014a1f8404e94f2d073f00
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04086227

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