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Potassium Iodide → (R)-N-(3-(3,3-bis(2-methylphenyl)-2-propen-1-yloxy)-1-propyl)3-piperidinecarboxylic acid ethyl ester

HRID 1614825
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HRID 1614825 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH3:22])=[CH:9][CH2:10][O:11][CH2:12][CH2:13][CH2:14]O.C([Li])CCC.C1(C)C=CC(S(Cl)(=O)=O)=CC=1.[NH:39]1[CH2:44][CH2:43][CH2:42][C@@H:41]([C:45]([O:47][CH2:48][CH3:49])=[O:46])[CH2:40]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C1(C)C=CC=CC=1.CC(C)=O>[CH2:48]([O:47][C:45]([C@@H:41]1[CH2:42][CH2:43][CH2:44][N:39]([CH2:14][CH2:13][CH2:12][O:11][CH2:10][CH:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:1])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])[CH2:40]1)=[O:46])[CH3:49]
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참가 물질

9

반응물 6

HCID 4875Potassium IodideHCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 185582ethyl (3R)-piperidine-3-carboxylateHCID 107563633-(3,3-Bis(2-methylphenyl)-2-propen-1-yloxy)-1-propanolHCID 178418339Butyllithium

생성물 1

HCID 54307972
(R)-N-(3-(3,3-bis(2-methylphenyl)-2-propen-1-yloxy)-1-propyl)3-piperidinecarboxylic acid ethyl ester
수율 52%

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 1140Toluene용매

실험 절차

A solution of 3-(3,3-bis(2-methylphenyl)-2-propen-1-yloxy)-1-propanol (3.45 g, 11.6 mmol) in dry toluene (150 ml) was cooled in an ice-bath and a solution of n-butyllithium in hexanes (5.1 ml, 2.5 M) was added dropwise. The reaction mixture was stirred for 15 minutes at room temperature and p-toluenesulphonyl chloride (2.44 g, 12.8 mmol) was added. The mixture was stirred at room temperature for 3 h. Ethyl (R)-3-piperidinecarboxylate (4.5 g, 23.3 mmol) and potassium carbonate (3.2 g, 23.3 mmol) were added and the mixture was stirred at room temperature for 0.5 h and then at 75° C. for 12 h. Potassium iodide (1.0 g) and acetone (40 ml) were added and the mixture was heated at reflux temperature for 15 h. Acetone (50 ml) was added and the cooled reaction mixture was filtered and the solvent evaporated in vacuo. Flash chromatography of the residue on silica gel (280 g) using a gradient of n-heptane in ethyl acetate as eluent afforded 2.6 g (52%) of (R)-N-(3-(3,3-bis(2-methylphenyl)-2-propen-1-yloxy)-1-propyl)3-piperidinecarboxylic acid ethyl ester as an oil. TLC: rf=0.52 (SiO2 ; methanol/ethyl acetate=1:9).

후처리

  1. stirringThe mixture was stirred at room temperature for 3 h
  2. stirringthe mixture was stirred at room temperature for 0.5 h
  3. waitat 75° C. for 12 h
  4. temperaturethe mixture was heated
  5. temperatureat reflux temperature for 15 h
  6. customthe cooled reaction mixture
  7. filtrationwas filtered
  8. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-4fb749d5b3e04d97a64e4845b1a63146
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05198451

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