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3-Methylmorpholine → 5-(3-Methylmorpholino)-2-morpholinopyridin-3-amine

HRID 1431524
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HRID 1431524 반응식
Br[C:2]1[CH:3]=[C:4]([NH2:14])[C:5]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][CH:7]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.[CH3:49][CH:50]1[CH2:55][O:54][CH2:53][CH2:52][NH:51]1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C>C1COCC1.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].O>[CH3:49][CH:50]1[N:51]([C:2]2[CH:3]=[C:4]([NH2:14])[C:5]([N:8]3[CH2:13][CH2:12][O:11][CH2:10][CH2:9]3)=[N:6][CH:7]=2)[CH2:52][CH2:53][O:54][CH2:55]1
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참가 물질

8

반응물 4

HCID 2921033-MethylmorpholineHCID 2733832Lithium hexamethyldisilazaneHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 467378735-Bromo-2-morpholinopyridin-3-amine

생성물 1

HCID 596314335-(3-Methylmorpholino)-2-morpholinopyridin-3-amine

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 8028Tetrahydrofuran용매2회

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온도
65 °C

실험 절차

To a stirred solution of 5-bromo-2-morpholinopyridin-3-amine (0.5 g, 1.94 mmol), dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (0.074 g, 0.16 mmol), Pd2dba3 (0.071 g, 0.08 mmol) and 3-methylmorpholine (0.98 g, 9.7 mmol) in THF (3.9 mL). To this mixture was added LHMDS in THF (1.0 M, 10.65 mL, 10.65 mmol) and the resulting reaction was heated to 65° C. The reaction was stirred for 2.25 h. After which, the reaction was cooled to rt and then poured into water (50 mL) and extracted with EtOAc (2×50 mL) and DCM (2×50 mL). The combined organic layers were dried over magnesium sulfate and the crude product was purified on basic alumina (0-100% EtOAc/hexane) to give 5-(3-methylmorpholino)-2-morpholinopyridin-3-amine. Mass Spectrum (ESI) m/e=279.2 (M+1).

후처리

  1. customthe resulting reaction
  2. temperatureAfter which, the reaction was cooled to rt
  3. extractionextracted with EtOAc (2×50 mL) and DCM (2×50 mL)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. customthe crude product was purified on basic alumina (0-100% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-19230917c8d04d4d98110c960c62ec92
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940724B2

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