Dimethylformamide → HCID 58746509、化合物

HRID 724724ノート

反応式

HRID 724724 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[I:30])[CH2:5][C@H:6]([NH:19][C:20](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[C:7](=O)[NH:8][CH2:9][C:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C([O-])(=O)C.[NH4+].C[N:37](C)C=O>O>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][C@H:6]([NH:19][C:20](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[C:7]2[NH:37][C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[CH:9][N:8]=2)[CH:27]=[CH:28][C:29]=1[I:30]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 517165Ammonium AcetateHCID 58746572tert-Butyl (1S)-1-(3-bromo-4-iodobenzyl)-2-oxo-2-[(2-oxo-2-phenylethyl)amino]ethylcarbamate

生成物 1

HCID 58746509HCID 58746509、化合物収率 38%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of tert-butyl (1S)-1-(3-bromo-4-iodobenzyl)-2-oxo-2-[(2-oxo-2-phenylethyl)amino]ethylcarbamate (1.20 g, 1.63 mmol), ammonium acetate (6.30 g, 81.7 mmol) and N,N-dimethylformamide (15.1 mL) was microwave irradiated at 120° C. for 30 min. The reaction was diluted with water and extracted with ethyl acetate three times, dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography to yield the desired product (440 mg, 38%).

後処理

  1. extractionextracted with ethyl acetate three times
  2. dry with materialdried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude residue was purified by flash column chromatography

出典と根拠

ORDレコード
ord-5103c16af907488b887e133dea37a39a
出典データセット
uspto-grants-2006_11
特許番号
US07141596B2

反応ノート

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