Sodium Chloride → 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-ol

HRID 2104984ノート

反応式

HRID 2104984 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([O:57][CH:58]([CH3:60])[CH3:59])[C:7]([F:56])=[C:8]([CH:10]([NH:43][C:44]2[CH:49]=[CH:48][C:47]([C:50]3[N:54]=[C:53]([CH3:55])[O:52][N:51]=3)=[CH:46][CH:45]=2)[C:11]2[N:12]([C:24]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH:13]=[C:14]([C:16]3[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=3[CH:18]=[O:19])[N:15]=2)[CH:9]=1)[CH3:2].[CH3:61][CH2:62][Mg+].[Br-].CCOC(C)=O.[Na+].[Cl-]>C1COCC1>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([O:57][CH:58]([CH3:59])[CH3:60])[C:7]([F:56])=[C:8]([CH:10]([NH:43][C:44]2[CH:45]=[CH:46][C:47]([C:50]3[N:54]=[C:53]([CH3:55])[O:52][N:51]=3)=[CH:48][CH:49]=2)[C:11]2[N:12]([C:24]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH:13]=[C:14]([C:16]3[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=3[CH:18]([OH:19])[CH2:61][CH3:62])[N:15]=2)[CH:9]=1)[CH3:2]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8857Ethyl AcetateHCID 866079362-(2-((5-ethoxy-2-fluoro-3-isopropoxyphenyl)(4-(5-methyl-1,2,4-oxadiazol-3-yl)phenylamino)methyl)-1-trityl-1H-imidazol-4-yl)benzaldehydeHCID 178461630HCID 178461630、化合物

生成物 1

HCID 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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of Intermediate 122.1 (50 mg, 0.06 mmol) in THF (1 mL) was added EtMgBr dropwise at 0° C. under N2 atmosphere, the reaction mixture was stirred at 0° C. for 30 min. The reaction mixture was then partionated between EtOAc and sat. NaCl, the organic layer was collected and dried over (Na2SO4), filtered and concentrated. The crude material Intermediate 122.2 was used as is in the following step. LCMS (2 min gradient) RT=2.23 min, 828.4 (M+H).

後処理

  1. customthe organic layer was collected
  2. dry with materialdried over (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customLCMS (2 min gradient) RT=2.23 min, 828.4 (M+H)

出典と根拠

ORDレコード
ord-02e3a39cfd894ebeae8266a847b3b507
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…