Sodium Carbonate → HCID 11582566, 화합물

HRID 1023792

반응식

HRID 1023792 반응식
B([C:4]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:5]=1[O:6][C@@H:7]([CH3:11])[C:8]([OH:10])=[O:9])(O)O.Br[C:18]1[CH:32]=[CH:31][C:21]([C:22]([N:24]([CH:28]([CH3:30])[CH3:29])[CH:25]([CH3:27])[CH3:26])=[O:23])=[C:20]([F:33])[CH:19]=1.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].O1CCOCC1>[CH3:27][CH:25]([N:24]([CH:28]([CH3:30])[CH3:29])[C:22]([C:21]1[CH:31]=[CH:32][C:18]([C:4]2[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:5]=2[O:6][C@@H:7]([CH3:11])[C:8]([OH:10])=[O:9])=[CH:19][C:20]=1[F:33])=[O:23])[CH3:26]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 672771854-bromo-2-fluoro-N,N-bis(1-methylethyl)-benzamideHCID 67277298(2S)-2-(2-borono-4-chlorophenoxy)-propanoic acid

생성물 1

HCID 11582566HCID 11582566, 화합물

시약·촉매·용매 2

HCID 178418228Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 312751,4-Dioxane용매

실험 절차

The product of step c) (200 mg), the product of step d) (200 mg), Pd(dppf)Cl2 (60 mg), sodium carbonate (350 mg) and dioxan (5 ml) were charged to a flask and heated at reflux for 24 h, then cooled to room temp and filtered (hyflo). The filtrate was concentrated in vacuo, then purified by reverse phase HPLC to give the title compound. Yield 22 mg

후처리

  1. temperatureheated
  2. temperatureat reflux for 24 h
  3. filtrationfiltered (hyflo)
  4. concentrationThe filtrate was concentrated in vacuo
  5. custompurified by reverse phase HPLC

출처 및 근거

ORD 기록
ord-bad716b28a464e43be1db3d9c312457c
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722741B2

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