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Cesium carbonate → HCID 57948966, 화합물

HRID 1992276
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HRID 1992276 반응식
Br[C:2]1[C:3]([F:17])=[CH:4][C:5]([F:16])=[C:6]([C@:8]2([CH3:15])[CH2:13][CH2:12][S:11][C:10]([NH2:14])=[N:9]2)[CH:7]=1.[N:18]1[CH:23]=[C:22](B(O)O)[CH:21]=[N:20][CH:19]=1.[C:27](=[O:30])([O-])[O-:28].[Cs+].[Cs+]>COCCOC.O.C(O)C.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[C:6]([O:28][C:27](=[O:30])[NH:14][C:10]1[S:11][CH2:12][CH2:13][C@:8]([C:6]2[CH:7]=[C:2]([C:22]3[CH:23]=[N:18][CH:19]=[N:20][CH:21]=3)[C:3]([F:17])=[CH:4][C:5]=2[F:16])([CH3:15])[N:9]=1)([CH3:8])([CH3:7])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 2795193(Pyrimidin-5-yl)boronic acidHCID 57948952HCID 57948952, 화합물

생성물 1

HCID 57948966HCID 57948966, 화합물수율 67%

시약·촉매·용매 3

HCID 178418476HCID 178418476, 화합물촉매HCID 962
Water
용매
HCID 86587095Dimethoxyethane ethanol water용매

실험 절차

To a 100° C. solution of (S)-4-(5-bromo-2,4-difluorophenyl)-4-methyl-5,6-dihydro-4H-1,3-thiazin-2-amine (12.6 g, 29.9 mmol, 1 equiv) in 1,2-dimethoxyethane:water:ethanol (15:7:5, 300 mL) is added a pyrimidine-5-boronic acid (25 g, 203 mmoles, 6.8 equiv) followed by cesium carbonate (58 g, 180 mmoles, 6 equiv) and bis(triphenylphosphine)palladium(II) chloride (4.2 g, 6.0 moles, 0.2 equiv). After 40 minutes, the reaction is cooled to ambient temperature, diluted with water, and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue is purified by silica gel chromatography eluting with a step gradient of hexanes:ethyl acetate (7:3) to hexanes:ethyl acetate (1:1) to give the title compound (67% yield): MS (m/z): 421 (M+1).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by silica gel chromatography
  6. washeluting with a step gradient of hexanes:ethyl acetate (7:3) to hexanes:ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-7627431c72394268b43f204e879b2454
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07648983B2

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