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Water → 6-{2-Cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethyl}-2-methoxy-3-methylpyridine

HRID 70613
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HRID 70613 반응식
C([Li])CCC.[CH3:6][O:7][C:8]1[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([S:22][CH3:23])=[CH:18][CH:17]=2)[N:9]=1.CC1C=CC(S(O[CH2:35][CH:36]2[CH2:40][CH2:39][CH2:38][CH2:37]2)(=O)=O)=CC=1.O>CCCCCC.O1CCCC1>[CH:36]1([CH2:35][CH:15]([C:10]2[N:9]=[C:8]([O:7][CH3:6])[C:13]([CH3:14])=[CH:12][CH:11]=2)[C:16]2[CH:17]=[CH:18][C:19]([S:22][CH3:23])=[CH:20][CH:21]=2)[CH2:40][CH2:39][CH2:38][CH2:37]1
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참가 물질

7

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HCID 962WaterHCID 12568544Cyclopentylmethyl 4-methylbenzene-1-sulfonateHCID 584525372-Methoxy-3-methyl-6-[4-(methylsulfanyl)benzyl]pyridineHCID 178418339Butyllithium

생성물 1

HCID 673994926-{2-Cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethyl}-2-methoxy-3-methylpyridine

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8058Hexane용매

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온도
-35 °C

실험 절차

A solution of 2.46 M n-butyllithium in hexane (1.11 mL) was added to a solution of 2-methoxy-3-methyl-6-[4-(methylsulfanyl)benzyl]pyridine obtained in Reference Example 2-1 (400 mg) in tetrahydrofuran (5 mL) in the presence of an argon gas at −78° C., and the mixture was stirred at −35° C. for 30 minutes. The reaction solution was cooled again to −78° C. and a solution of cyclopentylmethyl 4-methylbenzenesulfonate (549 mg) in tetrahydrofuran (3 mL) was added, after which the mixture was stirred at −78° C. to 0° C. for two hours. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by preparative TLC (hexane:ethyl acetate=19:1) to give 6-{2-cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethyl}-2-methoxy-3-methylpyridine as a colorless amorphous (220 mg, 42%).

후처리

  1. temperatureThe reaction solution was cooled again to −78° C.
  2. stirringafter which the mixture was stirred at −78° C. to 0° C. for two hours
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customThe solvent was then evaporated under reduced pressure
  8. customThe residue was purified by preparative TLC (hexane:ethyl acetate=19:1)

출처 및 근거

ORD 기록
ord-40d38caecfbb4e53a943959340faf1f6
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

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