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Sodium Carbonate → HCID 86679167, 화합물

HRID 1774813
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HRID 1774813 반응식
Br[C:2]1[CH:3]=[C:4]([C:8]2([C:11]([O-:13])=[O:12])[CH2:10][CH2:9]2)[CH:5]=[N:6][CH:7]=1.[K+].[CH3:15][N:16]1[C:25]2[C:20](=[CH:21][C:22](B3OC(C)(C)C(C)(C)O3)=[CH:23][CH:24]=2)[CH2:19][CH2:18][C:17]1=[O:35].C([O-])([O-])=O.[Na+].[Na+]>C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl.CN(C=O)C>[CH3:15][N:16]1[C:25]2[C:20](=[CH:21][C:22]([C:2]3[CH:3]=[C:4]([C:8]4([C:11]([OH:13])=[O:12])[CH2:10][CH2:9]4)[CH:5]=[N:6][CH:7]=3)=[CH:23][CH:24]=2)[CH2:19][CH2:18][C:17]1=[O:35]
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 66788306HCID 66788306, 화합물HCID 722082331-methyl-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3,4-dihydroquinolin-2(1H)-one

생성물 1

HCID 86679167HCID 86679167, 화합물수율 112.5%

시약·촉매·용매 2

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매
HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

A flask was charged with potassium 1-(5-bromopyridin-3-yl)cyclopropanecarboxylate (0.5 g, 1.52 mmol), 1-methyl-6-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3,4-dihydro-1H-quinolin-2-one (intermediate A-1, 0.479 g, 1.67 mmol) and DMF (7 mL). Then, bis(triphenylphosphine)palladium(II)chloride (0.106 g, 0.152 mmol), followed by 1N aqueous Na2CO3 solution (3.64 mL, 2.4 mmol) were added and the reaction was heated to 120° C. (pre-heated oil bath) for 1 h. The mixture was evaporated to dryness and the residue purified by silica gel flash chromatography eluting with a 0 to 15% MeOH-DCM gradient to give the title compound (0.551 g, 100%) as a brown solid. MS: 323.4 (M+H+).

후처리

  1. additionwere added
  2. temperature(pre-heated oil bath) for 1 h
  3. customThe mixture was evaporated to dryness
  4. customthe residue purified by silica gel flash chromatography
  5. washeluting with a 0 to 15% MeOH-DCM gradient

출처 및 근거

ORD 기록
ord-768dfcf5fe884cd4896590056650d50b
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09260408B2

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