Dimethylformamide → HCID 178500174、化合物

HRID 1513277ノート

反応式

HRID 1513277 の反応式
OOS([O-])=O.[K+].[CH3:7][O:8][C:9](=[O:24])[C:10]([CH3:23])([CH3:22])[CH2:11][C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([CH:19]=O)=[C:14]([CH3:21])[CH:13]=1.ClC1C=C(N[C:33]2[O:37][C:36]([C:38]3[CH:39]=[CH:40][C:41]4[N:45]=C(C5C(C)=CC(CCC(O)=O)=CC=5C)[NH:43][C:42]=4[CH:59]=3)=[N:35][N:34]=2)C=CC=1.CN([CH:63]=[O:64])C>O>[CH3:7][O:8][C:9](=[O:24])[C:10]([CH3:23])([CH3:22])[CH2:11][C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([C:19]2[NH:45][C:41]3[CH:40]=[CH:39][C:38]([C:36]4[O:37][C:33]([C:12]5[CH:17]=[CH:16][C:15]([O:64][CH3:63])=[CH:14][CH:13]=5)=[N:34][N:35]=4)=[CH:59][C:42]=3[N:43]=2)=[C:14]([CH3:21])[CH:13]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 23707502Potassium hydroxy sulfiteHCID 252105913-(4-{6-[5-(3-Chlorophenylamino)-[1,3,4]oxadiazol-2-yl]-1H-benzoimidazol-2-yl}-3,5-dimethylphenyl)-propionic acidHCID 86632822Methyl 3-(4-formyl-3,5-dimethylphenyl)-2,2-dimethylpropanoate

生成物 1

HCID 178500174HCID 178500174、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Oxone (420 mg, 0.683 mmol) was added to a mixture of 3-(4-formyl-3,5-dimethyl-phenyl)-2,2-dimethyl-propionic acid methyl ester (250 mg, 1.00 mmol) and 4-[5-(4-Methoxy-phenyl)-[1,3,4]oxadiazol-2-yl]-benzene-1,2-diamine (prepared as described in Example 1-59, 300 mg, 1.06 mmol) in DMF (8 mL) and water (0.8 mL), and the mixture was stirred at room temperature for 18 h. The mixture was partitioned between EtOAc and water. The EtOAc extract was washed with brine, dried over Na2SO4, concentrated and chromatographed to give the title compound. m/z 511.3 (MH+).

後処理

  1. customThe mixture was partitioned between EtOAc and water
  2. extractionThe EtOAc extract
  3. washwas washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customchromatographed

出典と根拠

ORDレコード
ord-08e483538d34419aa193382d6b9a763a
出典データセット
uspto-grants-2012_07
特許番号
US08217065B2

反応ノート

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