Tetrahydrofuran → HCID 45091887, 화합물

HRID 34104

반응식

HRID 34104 반응식
O1CCCC1.[BH4-].[Na+].[C:8]([O:12][C:13](=[O:31])[NH:14][CH:15]([C:26]1[O:27][CH:28]=[CH:29][N:30]=1)S(C1C=CC(C)=CC=1)(=O)=O)([CH3:11])([CH3:10])[CH3:9].[Cl-].[NH4+]>O>[C:8]([O:12][C:13](=[O:31])[NH:14][CH2:15][C:26]1[O:27][CH:28]=[CH:29][N:30]=1)([CH3:11])([CH3:9])[CH3:10]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 60034835[Oxazol-2-yl-(toluene-4-sulfonyl)-methyl]-carbamic Acid Tert-Butyl Ester

생성물 1

HCID 45091887HCID 45091887, 화합물수율 53.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 4 mL of tetrahydrofuran was added 51.4 mg of sodium borohydride, and added with 240 mg of [oxazole-2-yl-(toluene-4-sulfonyl)-methyl]-carbamic acid tert-butyl ester obtained by Production example 769 over 13 minutes at room temperature under stirring. Thereafter, the solution was stirred for another 2 hours and 30 minutes under room temperature, added with saturated aqueous ammonium chloride under ice cooling, and stirred for another 30 minutes under ice cooling. Thereafter, water was added, extracted twice with diethyl ether and dried over anhydrous magnesium sulfate. The solvent was evaporated, followed by purification and separation by silica gel column chromatography, to afford 72.3 mg of the title compound as colorless crystals.

후처리

  1. customobtained by Production example 769 over 13 minutes at room temperature
  2. stirringThereafter, the solution was stirred for another 2 hours and 30 minutes under room temperature
  3. stirringstirred for another 30 minutes under ice cooling
  4. extractionextracted twice with diethyl ether
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated
  7. customfollowed by purification and separation by silica gel column chromatography

출처 및 근거

ORD 기록
ord-c140664bf10945baae4d8b114ad87691
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429609B2

연결된 노트

불러오는 중…