2-Methyl-2-butene → HCID 178454342, 화합물

HRID 1875072노트

반응식

HRID 1875072 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][C:29]([CH:33]=[O:34])=[C:30]([Br:32])[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>[CH3:26][C:23]([O:22][C:20]([N:19]([C:17]([O:16][C:13]([CH3:12])([CH3:14])[CH3:15])=[O:18])[C:27]1[NH:28][C:29]([C:33]([OH:5])=[O:34])=[C:30]([Br:32])[N:31]=1)=[O:21])([CH3:24])[CH3:25]

참가 물질

8

반응물 4

HCID 105532-Methyl-2-buteneHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 23668197Sodium ChloriteHCID 178454341HCID 178454341, 화합물

생성물 1

HCID 178454342HCID 178454342, 화합물수율 30.1%

시약·촉매·용매 3

HCID 962Water용매HCID 6386tert-Butanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of sodium chlorite (0.348 g, 3.84 mmol) and sodium dihydrogenphosphate monohydrate (0.318 g, 2.306 mmol) in water (4 mL) was added to a solution of bis(1,1-dimethylethyl)(4-bromo-5-formyl-1H-imidazol-2-yl)imidodicarbonate (0.150 g, 0.384 mmol), 2-methyl-2-butene (2M in THF) (2.402 mL, 4.80 mmol), t-BuOH (2 mL) and THF (6 mL). The mixture was stirred at RT overnight and extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated. The residue was triturated with ether to give the desired product (0.047 g, 30%) as a white solid. ES MS: m/z 406 (M+1).

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was triturated with ether

출처 및 근거

ORD 기록
ord-03d9090abadb48d7b2f7f5ab1a5cfd75
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304419B2

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