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4-Methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline → 5-(5-amino-2-methylphenyl)-1-methyl-3-morpholinopyridin-2(1H)-one

HRID 594084
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HRID 594084 반응식
Br[C:2]1[CH:3]=[C:4]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:5](=[O:9])[N:6]([CH3:8])[CH:7]=1.[CH3:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][C:18]=1B1OC(C)(C)C(C)(C)O1>COCCOC.C(=O)([O-])[O-].[Na+].[Na+].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[NH2:21][C:20]1[CH:19]=[CH:18][C:17]([CH3:16])=[C:23]([C:2]2[CH:3]=[C:4]([N:10]3[CH2:15][CH2:14][O:13][CH2:12][CH2:11]3)[C:5](=[O:9])[N:6]([CH3:8])[CH:7]=2)[CH:22]=1
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참가 물질

6

반응물 2

HCID 160860894-Methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)anilineHCID 904089385-bromo-1-methyl-3-morpholinopyridin-2(1H)-one

생성물 1

HCID 904081725-(5-amino-2-methylphenyl)-1-methyl-3-morpholinopyridin-2(1H)-one수율 31%

시약·촉매·용매 3

HCID 178418807HCID 178418807, 화합물촉매HCID 8071
1,2-Dimethoxyethane
용매
HCID 10340Sodium Carbonate용매

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온도
120 °C

실험 절차

To a solution of 5-bromo-1-methyl-3-morpholinopyridin-2(1H)-one (1.0 equiv.) and 4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (1.2 equiv.) in DME and 2M sodium carbonate (3:1, 0.14 M) was added PdCl2(dppf)-DCM adduct (0.1 equiv.) in a microwave vial equipped with a stir bar. The reaction was heated to 120° C. for 15 min in the microwave. The solution was partitioned between water and ethyl acetate, the organic phase was dried with sodium sulfate, filtered and concentrated. The crude material was purified via silica gel column chromatography eluting with 100% ethyl acetate followed by 10% methanol in ethyl acetate. The pure fractions were concentrated and dried under vacuo to afford 5-(5-amino-2-methylphenyl)-1-methyl-3-morpholinopyridin-2(1H)-one in 31% yield. LCMS (m/z) (M+H)=300.2, Rt=0.41 min.

후처리

  1. customvial equipped with a stir bar
  2. customThe solution was partitioned between water and ethyl acetate
  3. dry with materialthe organic phase was dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified via silica gel column chromatography
  7. washeluting with 100% ethyl acetate
  8. concentrationThe pure fractions were concentrated
  9. customdried under vacuo

출처 및 근거

ORD 기록
ord-a229ebc32e34438fbf9a1118d1bf94fb
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242969B2

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