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 558959노트

반응식

HRID 558959 반응식
[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]

참가 물질

4

반응물 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

생성물 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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-4cec32232e0c435b9517a04fff59cd4a
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063038B2

반응 노트

불러오는 중…