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3-(Methylthio)-1-propanol → HCID 68971106, 화합물

HRID 540895
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HRID 540895 반응식
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[N:6]([CH2:19][CH2:20][CH3:21])[C:7]2[C:16]3[CH:15]=[CH:14][C:13]([OH:17])=[CH:12][C:11]=3[N:10]=[CH:9][C:8]=2[N:18]=1.C(OC1C=C(C=CC=1)N)C1C=CC=CC=1.COCCC(Cl)=O.C(OC1C=CC(N)=CC=1)C1C=CC=CC=1.C(OCC(Cl)=O)C.N(C(OC(C)C)=O)=NC(OC(C)C)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH3:99][S:100][CH2:101][CH2:102][CH2:103]O>O1CCCC1>[CH3:1][O:2][CH2:3][CH2:4][C:5]1[N:6]([CH2:19][CH2:20][CH3:21])[C:7]2[C:16]3[CH:15]=[CH:14][C:13]([O:17][CH2:103][CH2:102][CH2:101][S:100][CH3:99])=[CH:12][C:11]=3[N:10]=[CH:9][C:8]=2[N:18]=1
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참가 물질

10

반응물 8

HCID 104483-(Methylthio)-1-propanolHCID 11776TriphenylphosphineHCID 228604-BenzyloxyanilineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 84189Ethoxyacetyl chlorideHCID 928923-BenzyloxyanilineHCID 27597283-Methoxypropanoyl chloride
HCID 136347851
HCID 136347851, 화합물
2회

생성물 1

HCID 68971106HCID 68971106, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

A modification on the methods described in Parts A-H of Example 2 were used to prepare 2-(2-methoxyethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-7-ol, with 3-benzyloxyaniline and 3-methoxypropanoyl chloride used in lieu of 4-benzyloxyaniline and ethoxyacetyl chloride, respectively. Diisopropyl azodicarboxylate (2.07 mL, 10.5 mmol) was added dropwise to a slurry of 2-(2-methoxyethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-7-ol (2.00 g, 7.01 mmol), triphenylphosphine (2.75 g, 10.5 mmol), and 3-(methylthio)propan-1-ol (1.08 mL, 10.5 mmol) in tetrahydrofuran (70 mL) at 0° C. The solution was stirred for 30 minutes at 0° C., then at room temperature for 16 hours. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate, treated with 1 M hydrochloric acid (40 mL), and stirred for 30 minutes. The layers were separated and the aqueous layer was extracted with ethyl acetate (2×25 mL). The aqueous layer was adjusted to approximately pH 14 with 50% aqueous sodium hydroxide and then was extracted with dichloromethane (3×50 mL). The organic layers were combined, washed with water and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by flash chromatography (silica gel, gradient elution with 1-4% methanol in dichloromethane) to provide 2.0 g of 2-(2-methoxyethyl)-7-[3-(methylthio)propoxy]-1-propyl-1H-imidazo[4,5-c]quinoline as an opaque solid.

후처리

  1. waitat room temperature for 16 hours
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. additiontreated with 1 M hydrochloric acid (40 mL)
  5. stirringstirred for 30 minutes
  6. customThe layers were separated
  7. extractionthe aqueous layer was extracted with ethyl acetate (2×25 mL)
  8. extractionwas extracted with dichloromethane (3×50 mL)
  9. washwashed with water and saturated aqueous sodium chloride
  10. dry with materialdried over anhydrous sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. customThe crude product was purified by flash chromatography (silica gel, gradient elution with 1-4% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-dd5920661b3d4c2198c1240434a1d2e8
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871782B2

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