Imidazole → HCID 54284754, 화합물

HRID 2291292노트

반응식

HRID 2291292 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].N1C=CN=C1.[C:16]1([Si:22](Cl)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:23]([CH3:26])([CH3:25])[CH3:24])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CN(C)C=O>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][Si:22]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:23]([CH3:26])([CH3:24])[CH3:25])=[O:6]

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 74203-Hydroxybenzoic AcidHCID 94078tert-Butyldiphenylchlorosilane

생성물 1

HCID 54284754HCID 54284754, 화합물수율 52.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To stirred solution of 50.4 g of 3-hydroxybenzoic acid in 200 ml of dry dimethylformamide at 0° C. was added 24.85 g of imidazole, followed by 100 g of diphenyl-(2-methylprop-2-yl)silyl chloride. The mixture was stirred at room temperature for 16 hours, and partitioned between ethyl acetate and cold water. The organic layer was washed with water, with an aqueous potassium hydrogen carbonate solution and with brine, was dried over anhydrous magnesium sulphate and evaporated to dryness. The resulting white solid was slurried in dry chloroform and filtered to afford 72 g of the title compound.

후처리

  1. custompartitioned between ethyl acetate and cold water
  2. washThe organic layer was washed with water, with an aqueous potassium hydrogen carbonate solution and with brine
  3. dry with materialwas dried over anhydrous magnesium sulphate
  4. customevaporated to dryness
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-9e8ffa4e6b3c4722a96061e80dbc1af1
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04795748

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