2-Methyl-2-butene → HCID 178524893, 화합물

HRID 43459

반응식

HRID 43459 반응식
[OH2:1].O.P([O-])(O)(O)=O.[Na+].CC(=CC)C.Cl([O-])=O.[Na+].[F:18][C:19]([F:28])([F:27])[C:20]1[N:21]=[C:22]([CH:25]=[O:26])[NH:23][CH:24]=1>C(O)(C)(C)C>[F:28][C:19]([F:18])([F:27])[C:20]1[N:21]=[C:22]([C:25]([OH:1])=[O:26])[NH:23][CH:24]=1

참가 물질

6

반응물 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23673460Sodium Phosphate, Monobasic, DihydrateHCID 178519985HCID 178519985, 화합물

생성물 1

HCID 178524893HCID 178524893, 화합물수율 98%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

Sodium dihydrogenphosphate dihydrate (720 mg, 4.62 mmol), 2-methyl-2-butene (1.2 ml, 11.4 mmol) and sodium chlorite (420 mg, 4.64 mmol) were added under ice-cooling to a solution of 4-(trifluoromethyl)-1H-imidazole-2-carbaldehyde obtained in Example (33b) (375 mg, 2.29 mmol) in t-butyl alcohol (12 ml)/distilled water (5 ml), followed by stirring for 1.5 hours. The reaction solution was concentrated under reduced pressure, and then the residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water) to obtain 0.402 g of the title compound as a white solid (98%).

후처리

  1. distillation)/distilled water (5 ml)
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. distillationthe residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water)

출처 및 근거

ORD 기록
ord-dfb5dbc140d94e42ae20fad4d81cbb8b
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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