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 1873272노트

반응식

HRID 1873272 반응식
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]

참가 물질

4

반응물 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

생성물 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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a9168172cf924a5e8f1d3882d320a3ec
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06110946

반응 노트

불러오는 중…