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Morpholine → Methyl 5-morpholinonicotinate

HRID 1174511
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HRID 1174511 반응식
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[C:8](Br)[CH:7]=[N:6][CH:5]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C1(C)C=CC=CC=1.C(OCC)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>[N:12]1([C:8]2[CH:7]=[N:6][CH:5]=[C:4]([CH:9]=2)[C:3]([O:2][CH3:1])=[O:11])[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1
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참가 물질

7

반응물 2

HCID 8083MorpholineHCID 699336Methyl 5-bromopyridine-3-carboxylate

생성물 1

HCID 355238Methyl 5-morpholinonicotinate수율 42%

시약·촉매·용매 4

HCID 634876Binap, (A+-)-촉매HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 1140
Toluene
용매
HCID 3283Diethyl Ether용매

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온도
110 °C

실험 절차

To a mixture of methyl-5-bromonicotinate (10 g, 0.045 mol) and morpholine (4.6 g, 0.054 mol) in dry toluene (100 mL) was added fused CsCO3 (30 g, 0.09 mol) with stirring under argon. To this mixture was added BINAP (0.45 g, 0.0005 mol), Pd2(dba)3 (0.22 g, 0.00015 mol) and then the reaction mixture was refluxed at 110° C. for 50 h. The reaction mixture was cooled down to r.t. and diluted with diethyl ether (400 ml) and filtered through celite. The filtrate was concentrated under vacuum and purified by flash column chromatography (CHCl3/MeOH, 4:1) to give 4.2 g (41%) of methyl 5-morpholin-4-ylnicotinate as a liquid. TLC—Chloroform/Methanol (8/2): Rf=0.7.

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was cooled down to r.t.
  3. filtrationfiltered through celite
  4. concentrationThe filtrate was concentrated under vacuum
  5. custompurified by flash column chromatography (CHCl3/MeOH, 4:1)

출처 및 근거

ORD 기록
ord-e86a4f1f9e3844ab99f10bcba60ae2eb
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07838522B2

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