Imidazole → HCID 58014000, 화합물

HRID 2357899노트

반응식

HRID 2357899 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:13]=[C:6]2[C:7]([CH2:11][OH:12])=[CH:8][CH:9]=[CH:10][N:5]2[N:4]=1.N1C=CN=C1.[Si:21](Cl)([C:24]([CH3:27])([CH3:26])[CH3:25])([CH3:23])[CH3:22].O>CN(C=O)C>[Si:21]([O:12][CH2:11][C:7]1[C:6]2[N:5]([N:4]=[C:3]([C:2]([F:1])([F:14])[F:15])[CH:13]=2)[CH:10]=[CH:9][CH:8]=1)([C:24]([CH3:27])([CH3:26])[CH3:25])([CH3:23])[CH3:22]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 59389331HCID 59389331, 화합물

생성물 1

HCID 58014000HCID 58014000, 화합물수율 43.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The compound of Example 64 (5.17 g, crude product) was dissolved in DMF (100 mL). To this solution, imidazole (4.89 g) and t-butyldimethylsilyl chloride (4.33 g) were added and the mixture was stirred at room temperature for 1.5 hours. Subsequently, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate. Evaporation of the solvent and subsequent purification by silica gel column chromatography (hexane:ethyl acetate=9:1) afforded the title compound as a yellow oil (3.42 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed sequentially with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customEvaporation of the solvent and subsequent purification by silica gel column chromatography (hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-f315cbb500dd4fd28e83a5e8fc40e0fb
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763617B2

반응 노트

불러오는 중…