Triacetoxyperiodinane → 8-Fluoro-3-oxo-4-(2-oxoethyl)-3,4-dihydro-2H-quinoxaline-1-carboxylic acid 2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylamide

HRID 558959ノート

反応式

HRID 558959 の反応式
[CH3:1][C:2]1[CH:26]=[C:25]([C:27]([N:29]2[CH2:35][CH2:34][CH2:33][CH2:32][C:31]3[CH:36]=[CH:37][CH:38]=[CH:39][C:30]2=3)=[O:28])[CH:24]=[CH:23][C:3]=1[CH2:4][NH:5][C:6]([N:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][C:16]=2[F:18])[N:11]([CH2:19][CH2:20][OH:21])[C:10](=[O:22])[CH2:9]1)=[O:7].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>ClCCl>[CH3:1][C:2]1[CH:26]=[C:25]([C:27]([N:29]2[CH2:35][CH2:34][CH2:33][CH2:32][C:31]3[CH:36]=[CH:37][CH:38]=[CH:39][C:30]2=3)=[O:28])[CH:24]=[CH:23][C:3]=1[CH2:4][NH:5][C:6]([N:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][C:16]=2[F:18])[N:11]([CH2:19][CH:20]=[O:21])[C:10](=[O:22])[CH2:9]1)=[O:7]

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 115482588-Fluoro-4-(2-hydroxyethyl)-3-oxo-3,4-dihydro-2H-quinoxaline-1-carboxylic acid 2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylamide

生成物 1

HCID 115338268-Fluoro-3-oxo-4-(2-oxoethyl)-3,4-dihydro-2H-quinoxaline-1-carboxylic acid 2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 8-fluoro-4-(2-hydroxyethyl)-3-oxo-3,4-dihydro-2H-quinoxaline-1-carboxylic acid 2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylamide from Example 9 (105 mg, 0.20 mmol) in dichloromethane (5 ml) was added Dess-Martin periodinane (100 mg, 0.24 mg). The mixture was stirred for 2 h and evaporated. The residue was taken up in chloroform and water and separated. The organic layer was dried and evaporated. The residue was purified by flash chromatography on silica (eluant methanol:dichloromethane 4:96) to give a white solid; yield 73 mg, 69%.

後処理

  1. customevaporated
  2. customwater and separated
  3. customThe organic layer was dried
  4. customevaporated
  5. customThe residue was purified by flash chromatography on silica (eluant methanol:dichloromethane 4:96)
  6. customto give a white solid

出典と根拠

ORDレコード
ord-4cec32232e0c435b9517a04fff59cd4a
出典データセット
uspto-grants-2011_11
特許番号
US08063038B2

反応ノート

読み込み中…