Cesium carbonate → HCID 21137722、化合物

HRID 1358580ノート

反応式

HRID 1358580 の反応式
[CH3:1][O:2][C:3](=[O:28])[C@H:4]([CH2:20]C1C=CC(O)=CC=1)[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12](=[O:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Br[CH2:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32].C(=O)([O-])[O-:39].[Cs+].[Cs+]>CC(C)=O>[CH3:1][O:2][C:3](=[O:28])[C@H:4]([CH3:20])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:39][CH2:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])=[CH:8][C:7]=1[C:12](=[O:19])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 79177tert-Butyl bromoacetateHCID 10667178N-(2-benzoylphenyl)tyrosine methyl ester

生成物 1

HCID 21137722HCID 21137722、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of N-(2-benzoylphenyl)tyrosine methyl ester (0.97 g), t-butyl bromoacetate (0.55 ml), cesium carbonate (1.14 g), and acetone (15 ml) was stirred at room temperature for 1.5 hours and allowed to stand overnight. The reaction mixture was partitioned between ethyl acetate and water. The extract was washed with saturated aqueous chloride solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford the title compound (1.42 g, Rf=0.65: thin layer chromatography on a silica gel plate using hexane: ethyl acetate=3:1 as the eluant).

後処理

  1. waitto stand overnight
  2. customThe reaction mixture was partitioned between ethyl acetate and water
  3. washThe extract was washed with saturated aqueous chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1963ac32b3a04352b8a8fc389959067b
出典データセット
uspto-grants-2003_07
特許番号
US06596751B2

反応ノート

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