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Hydrochloric Acid → 1'-benzyl-6-ethylspiro[isobenzofuran-1(3H),4'-piperidine]-3-one hydrochloride

HRID 392806
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HRID 392806 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[O:10]CC(C)(C)N=2)=[CH:5][CH:4]=1)[CH3:2].CCCCCC.C([Li])CCC.[CH2:27]([N:34]1[CH2:39][CH2:38][C:37](=[O:40])[CH2:36][CH2:35]1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[ClH:41].[OH-].[Na+]>O1CCCC1>[ClH:41].[CH2:27]([N:34]1[CH2:39][CH2:38][C:37]2([C:7]3[C:6](=[CH:5][CH:4]=[C:3]([CH2:1][CH3:2])[CH:8]=3)[C:9](=[O:10])[O:40]2)[CH2:36][CH2:35]1)[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 192201-Benzyl-4-piperidoneHCID 128725592-(4-Ethylphenyl)-4,4-dimethyl-2-oxazolineHCID 178418244HCID 178418244, 화합물

생성물 1

HCID 226607251'-benzyl-6-ethylspiro[isobenzofuran-1(3H),4'-piperidine]-3-one hydrochloride

시약·촉매·용매

1
HCID 8028Tetrahydrofuran용매

실험 절차

Under a nitrogen atmosphere, a solution of 2-(4-ethylphenyl)-4,4-dimethyl-2-oxazoline (1.15 g) in anhydrous tetrahydrofuran (100 mL) was cooled to −78° C. To this solution was added 1.5 M butyl lithium hexane solution (4.53 mL). After being stirred for 1 hour, 1-benzyl-4-piperidone (1.05 mL) was added dropwise. After the reaction temperature was allowed to rise up to room temperature, 2N hydrochloric acid was added to the reaction mixture to make the mixture acidic. The whole was refluxed for 2 hours. After cooling, sodium hydroxide aqueous solution was added to make the reaction mixture basic. The mixture was extracted with ethyl ether. The organic layer was washed with saturated saline solution and then dried over anhydrous Na2SO4. The concentration of the organic solvent left a residue, which was purified by column chromatography on silica gel (hexane/ethyl acetate/=3/2) to give the subject compound (409 mg).

후처리

  1. customto rise up to room temperature
  2. temperatureThe whole was refluxed for 2 hours
  3. temperatureAfter cooling
  4. extractionThe mixture was extracted with ethyl ether
  5. washThe organic layer was washed with saturated saline solution
  6. dry with materialdried over anhydrous Na2SO4
  7. waitThe concentration of the organic solvent left a residue, which
  8. customwas purified by column chromatography on silica gel (hexane/ethyl acetate/=3/2)

출처 및 근거

ORD 기록
ord-e8321f610e0a4d0583fed708ad8b4ad9
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06803372B2

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