Dimethylformamide → HCID 178500174、化合物

HRID 1360781ノート

反応式

HRID 1360781 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-cb1966aa095c43a7b760958a6abbfdb6
出典データセット
uspto-grants-2011_02
特許番号
US07879850B2

反応ノート

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