Potassium Carbonate → HCID 59304991、化合物

HRID 2240252ノート

反応式

HRID 2240252 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[N:8]([S:12]([C:15]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=3)(=[O:14])=[O:13])[CH:9]=[C:10]([F:11])[C:3]=12.[F:22][C:23]1[CH:29]=[C:28]([N+:30]([O-:32])=[O:31])[CH:27]=[CH:26][C:24]=1[NH2:25].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.C(=O)([O-])[O-].[K+].[K+]>C(O)(C)(C)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:11][C:10]1[C:3]2[C:2]([NH:25][C:24]3[CH:26]=[CH:27][C:28]([N+:30]([O-:32])=[O:31])=[CH:29][C:23]=3[F:22])=[CH:7][CH:6]=[N:5][C:4]=2[N:8]([S:12]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)(=[O:14])=[O:13])[CH:9]=1

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 1012542-Fluoro-4-nitroanilineHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 497590784-Chloro-3-fluoro-1-(4-methylbenzene-1-sulfonyl)-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 59304991HCID 59304991、化合物

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 6386tert-Butanol溶媒

実験手順

A solution of 20 mg (0.06 mmol) of 4-chloro-3-fluoro-1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo[2,3-b]pyridine, 11.5 mg (0.074 mmol) of 2-fluoro-4-nitroaniline, 5.6 mg (0.006 mmol) of tris(dibenzylideneacetone)dipalladium, 5.8 mg (0.012 mmol) of dicyclohexyl(2′,4′,6′-triisopropyl-biphenyl-2-yl)phosphine and 12.7 mg (0.09 mmol) of potassium carbonate in 1.00 ml of degassed tert-butanol is stirred in a sealed pressure vessel at 100° C. for 3 h. After cooling to RT, the reaction mixture is filtered through kieselguhr, the kieselguhr is washed with ethyl acetate and the solvent is removed from the filtrate. The residue is purified by preparative HPLC.

後処理

  1. filtrationthe reaction mixture is filtered through kieselguhr
  2. washthe kieselguhr is washed with ethyl acetate
  3. customthe solvent is removed from the filtrate
  4. customThe residue is purified by preparative HPLC

出典と根拠

ORDレコード
ord-7335327f794c4aa0ae58f91ad60e77c2
出典データセット
uspto-grants-2010_05
特許番号
US07723347B2

反応ノート

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