2-Methyl-2-butene → HCID 178454351, 화합물

HRID 1875077노트

반응식

HRID 1875077 반응식
Cl([O-])=O.[Na+].[OH2:5].P([O-])(O)(O)=O.[Na+].[CH3:12][C:13]([O:16][C:17]([N:19]([C:27]1[NH:28][CH:29]=[C:30]([CH:32]=[O:33])[N:31]=1)[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])=[O:18])([CH3:15])[CH3:14].CC(=CC)C>O.C1COCC1.CC(O)(C)C>[CH3:15][C:13]([O:16][C:17]([N:19]([C:20]([O:22][C:23]([CH3:24])([CH3:25])[CH3:26])=[O:21])[C:27]1[NH:28][CH:29]=[C:30]([C:32]([OH:5])=[O:33])[N:31]=1)=[O:18])([CH3:12])[CH3:14]

참가 물질

8

반응물 4

HCID 105532-Methyl-2-buteneHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 23668197Sodium ChloriteHCID 178454349HCID 178454349, 화합물

생성물 1

HCID 178454351HCID 178454351, 화합물수율 53.6%

시약·촉매·용매 3

HCID 962Water용매HCID 6386tert-Butanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of sodium chlorite (0.505 g, 5.59 mmol) and sodium dihydrogenphosphate monohydrate (0.463 g, 3.35 mmol) in water (4 mL) was added to a solution of bis(1,1-dimethylethyl)(4-formyl-1H-imidazol-2-yl)imidodicarbonate (0.174 g, 0.559 mmol), 2-methyl-2-butene (2M in THF) (3.49 mL, 6.99 mmol), t-BuOH (2 mL) and THF (6 mL). The mixture was stirred at RT overnight. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated. The residue was triturated with ether and the resulting white solid was dried under vacuum to give 0.098 g (53%) of the title compound. MS m/z 326 (M−1).

후처리

  1. extractionThe reaction mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was evaporated
  4. customThe residue was triturated with ether
  5. customthe resulting white solid was dried under vacuum

출처 및 근거

ORD 기록
ord-aad38660bad042f0a60e49009d4d24f6
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304419B2

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