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Morpholine → Methyl 6-morpholinonicotinate

HRID 1878571
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HRID 1878571 반응식
Cl[C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>CO>[N:12]1([C:2]2[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=2)[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1
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참가 물질

4

반응물 2

HCID 8083MorpholineHCID 254249Methyl 6-chloropyridine-3-carboxylate

생성물 1

HCID 2776466Methyl 6-morpholinonicotinate수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

There was dissolved, in methanol (50 mL), methyl 6-chloro-nicotinate (4.00 g, 23.3 mM), then morpholine (6.10 mL, 69.9 mM) was added to the solution and the solution was stirred for 14 hours while refluxing the same with heating. The solvent was distilled off from this reaction liquid, the resulting residue was diluted with water and then extracted with ethyl acetate. The resulting extracts were combined, dried over anhydrous sodium sulfate, the solvent was distilled off to thus obtain methyl 6-(morpholin-4-yl)-nicotinate (4.07 g, yield: 79%). Subsequently, acetonitrile (1.61 mL, 30.6 mM) was added to a solution of 18-crown-6 (476 mg, 1.80 mM) and potassium tert-butoxide (1M THF solution, 27.0 mL, 27.0 mM) in THF (10 mL) at 60° C. and then the mixture was stirred for 5 minutes. To this solution, there was added the methyl 6-(morpholin-4-yl)-nicotinate (4.00 g, 18.0 mM) prepared above and the mixture was stirred for 30 minutes. This suspension was filtered and the resulting solid was washed with diethyl ether.

후처리

  1. temperaturewhile refluxing the same
  2. temperaturewith heating
  3. distillationThe solvent was distilled off from this reaction liquid
  4. additionthe resulting residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. dry with materialdried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-915fe67197624ea2becb1eac46aed5c5
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08314098B2

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