Ethyl Acetate → 1-(2-(2-((5-ethoxy-2-fluoro-3-isopropoxyphenyl)(4-(5-methyl-1,2,4-oxadiazol-3-yl)phenylamino)methyl)-1-trityl-1H-imidazol-4-yl)phenyl)propan-1-one

HRID 2104985ノート

反応式

HRID 2104985 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([O:59][CH:60]([CH3:62])[CH3:61])[C:7]([F:58])=[C:8]([CH:10]([NH:45][C:46]2[CH:51]=[CH:50][C:49]([C:52]3[N:56]=[C:55]([CH3:57])[O:54][N:53]=3)=[CH:48][CH:47]=2)[C:11]2[N:12]([C:26]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH:13]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH:22]([OH:25])[CH2:23][CH3:24])[N:15]=2)[CH:9]=1)[CH3:2].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.CCOC(C)=O.[OH-].[Na+]>C(Cl)Cl>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([O:59][CH:60]([CH3:62])[CH3:61])[C:7]([F:58])=[C:8]([CH:10]([NH:45][C:46]2[CH:51]=[CH:50][C:49]([C:52]3[N:56]=[C:55]([CH3:57])[O:54][N:53]=3)=[CH:48][CH:47]=2)[C:11]2[N:12]([C:26]([C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:39]3[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=3)[CH:13]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22](=[O:25])[CH2:23][CH3:24])[N:15]=2)[CH:9]=1)[CH3:2]

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 159087TriacetoxyperiodinaneHCID 688125741-(2-(2-((5-ethoxy-2-fluoro-3-isopropoxyphenyl)(4-(5-methyl-1,2,4-oxadiazol-3-yl)phenylamino)methyl)-1-trityl-1H-imidazol-4-yl)phenyl)propan-1-ol

生成物 1

HCID 688132671-(2-(2-((5-ethoxy-2-fluoro-3-isopropoxyphenyl)(4-(5-methyl-1,2,4-oxadiazol-3-yl)phenylamino)methyl)-1-trityl-1H-imidazol-4-yl)phenyl)propan-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of Intermediate 122.2 and Dess-Martin periodinate (60 mg, 0.12 mmol) in anhydrous CH2Cl2 (2 mL) was stirred at rt for 20 min. The reaction mixture was then partionated between EtOAc and 1 N NaOH, the organic layer was collected and dried over (Na2SO4), filtered and concentrated to afford Intermediate 122.3, which was used in the following step without further purification. LCMS (2 min gradient) RT=2.27 min, 826.4 (M+H).

後処理

  1. customthe organic layer was collected
  2. dry with materialdried over (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-fc281341685d4b629e7dc58c371263d1
出典データセット
uspto-grants-2009_08
特許番号
US07576098B2

反応ノート

読み込み中…