Potassium Carbonate → 1-{4-[2-(1-Methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-phenyl}-4(S)-hydroxy-2-(tert-butoxycarbonyl)amino-5(S)-amino-6-phenyl-2-azahexane

HRID 1873272ノート

反応式

HRID 1873272 の反応式
C([O-])([O-])=O.[K+].[K+].[CH3:7][C:8]([N:16]1[N:20]=[N:19][C:18]([C:21]2[CH:26]=[CH:25][C:24]([CH2:27][N:28]([NH:47][C:48]([O:50][C:51]([CH3:54])([CH3:53])[CH3:52])=[O:49])[CH2:29][C@H:30]([OH:46])[C@@H:31]([NH:39]C(=O)C(F)(F)F)[CH2:32][C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:23][CH:22]=2)=[N:17]1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:9]>CO>[CH3:9][C:8]([N:16]1[N:20]=[N:19][C:18]([C:21]2[CH:26]=[CH:25][C:24]([CH2:27][N:28]([NH:47][C:48]([O:50][C:51]([CH3:54])([CH3:53])[CH3:52])=[O:49])[CH2:29][C@H:30]([OH:46])[C@@H:31]([NH2:39])[CH2:32][C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:23][CH:22]=2)=[N:17]1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:7]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 229404541-{4-[2-(1-methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-phenyl}-4(S)-hydroxy-2-(tert-butoxycarbonyl)amino-5(S)-(trifluoroacetyl)amino-6-phenyl-2-azahexane

生成物 1

HCID 229404511-{4-[2-(1-Methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-phenyl}-4(S)-hydroxy-2-(tert-butoxycarbonyl)amino-5(S)-amino-6-phenyl-2-azahexane

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

28 ml of a 1N K2CO3 solution are added dropwise, at 70° C., to 1.9 g (2.8 mmol) of 1-{4-[2-(1-methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-phenyl}-4(S)-hydroxy-2-(tert-butoxycarbonyl)amino-5(S)-(trifluoroacetyl)amino-6-phenyl-2-azahexane in 29 ml of methanol and the mixture is stirred for 15 hours. After cooling and concentration by evaporation, methylene chloride and water and added; the aqueous phase is separated off and extracted with methylene chloride. The organic phases are washed with water, dried (Na2SO4) and concentrated by evaporation to yield the title compound: HPLC20-100 : tRet =15.1; FAB MS (M+H)+ =469.

後処理

  1. temperatureAfter cooling
  2. concentrationconcentration
  3. customby evaporation, methylene chloride and water
  4. additionadded
  5. customthe aqueous phase is separated off
  6. extractionextracted with methylene chloride
  7. washThe organic phases are washed with water
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-a9168172cf924a5e8f1d3882d320a3ec
出典データセット
uspto-grants-2000_08
特許番号
US06110946

反応ノート

読み込み中…