Triacetoxyperiodinane → HCID 136146894、化合物

HRID 1674410ノート

反応式

HRID 1674410 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-3ef294ea65054656b10142e81e00c97a
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

読み込み中…