Triacetoxyperiodinane → HCID 136146894、化合物

HRID 1719079ノート

反応式

HRID 1719079 の反応式
[CH2:1]([C:3]1[N:8]=[C:7]([CH2:9][CH2:10][CH3:11])[N:6]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]3[NH:29][C:28](=[O:30])[O:27][N:26]=3)=[CH:15][CH:14]=2)[C:5](=[O:31])[C:4]=1[C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[O:38][C:37]([CH3:43])([CH3:42])[CH2:36][CH:35]2[OH:44])[CH3:2].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C1=CC=CC=2)=O>ClCCl.C(OCC)(=O)C>[CH3:43][C:37]1([CH3:42])[CH2:36][C:35](=[O:44])[C:34]2[C:39](=[CH:40][CH:41]=[C:32]([C:4]3[C:5](=[O:31])[N:6]([CH2:12][C:13]4[CH:18]=[CH:17][C:16]([C:19]5[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=5[C:25]5[NH:29][C:28](=[O:30])[O:27][N:26]=5)=[CH:15][CH:14]=4)[C:7]([CH2:9][CH2:10][CH3:11])=[N:8][C:3]=3[CH2:1][CH3:2])[CH:33]=2)[O:38]1

参加物

5

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 136146825HCID 136146825、化合物

生成物 1

HCID 136146894HCID 136146894、化合物収率 81%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 6-ethyl-5-(4-hydroxy-2,2-dimethyl-3,4-dihydro-2H-chromen-6-yl)-3-{[2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}-2-propylpyrimidin-4(3H)-one (0.78 g) and 1,1,1-tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3(1H)-one (0.84 g) in dichloromethane (8 mL) was stirred for 1 hr. The reaction mixture was diluted with ethyl acetate, washed with water, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.63 g, 81%).

後処理

  1. washwashed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-140e139ac169443282772f39459fc333
出典データセット
uspto-grants-2010_09
特許番号
US07803940B2

反応ノート

読み込み中…