Sodium Carbonate → HCID 11582566、化合物

HRID 1023792

反応式

HRID 1023792 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 11582566HCID 11582566、化合物

試薬・触媒・溶媒 2

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

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-bad716b28a464e43be1db3d9c312457c
出典データセット
uspto-grants-2014_05
特許番号
US08722741B2

関連ノート

読み込み中…