Water → HCID 67170480、化合物

HRID 545106ノート

反応式

HRID 545106 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[Cl:22])[CH2:6][N:7]1[CH2:12][CH2:11][O:10][C@@H:9]([CH2:13][NH:14][C:15](=[O:18])[CH2:16]Cl)[CH2:8]1.[CH2:23]([O:25][C:26]([C:28]1[N:29]=[C:30]([SH:33])[S:31][CH:32]=1)=[O:27])[CH3:24].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[Cl:22])[CH2:6][N:7]1[CH2:12][CH2:11][O:10][C@@H:9]([CH2:13][NH:14][C:15](=[O:18])[CH2:16][S:33][C:30]2[S:31][CH:32]=[C:28]([C:26]([O:25][CH2:23][CH3:24])=[O:27])[N:29]=2)[CH2:8]1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 67169608HCID 67169608、化合物HCID 178470113HCID 178470113、化合物

生成物 1

HCID 67170480HCID 67170480、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The resultant product (776 mg) of (1-2) and the resultant product (379 mg) of (1-3) were dissolved in dimethylformamide (6 mL), potassium carbonate (829 mg) was added, and the mixture was stirred overnight at room temperature. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography using a mixed solvent of chloroform and methanol as an eluent. The solvent was evaporated from the eluent to give the title compound (850 mg) as a pale-yellow oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography
  6. customThe solvent was evaporated from the eluent

出典と根拠

ORDレコード
ord-edd85d36a50f4a5cb837aabd0e0ef1b9
出典データセット
uspto-grants-2011_05
特許番号
US07935700B2

反応ノート

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