Sodium Bicarbonate → HCID 85787172, 화합물

HRID 1865383노트

반응식

HRID 1865383 반응식
Br[CH:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[C:3](=O)[C:4]([CH3:7])([CH3:6])[CH3:5].[NH2:15][C:16]([NH2:18])=[S:17].C(=O)([O-])O.[Na+]>C(O)C>[NH2:18][C:16]1[S:17][C:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:3]([C:4]([CH3:7])([CH3:6])[CH3:5])[N:15]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 546382Bromo-dipivaloylmethaneHCID 2723790Thiourea

생성물 1

HCID 85787172HCID 85787172, 화합물수율 94.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4-bromo-2,2,6,6-tetramethyl-3,5-heptanedione (α-bromo-dipivaloylmethane; 1.42 g, 5.40 mmol), thiourea(451.8 mg, 5.94 mmol) and ethanol(15 mL) was refluxed for 2 hours. After the reaction mixture was cooled to room temperature, it was poured into saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate. After the ethyl acetate layer was washed successively with water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was crystallized by dichloromethane/n-hexane to give the title compound(1.23 g, 94.5%) as a white crystal.

후처리

  1. temperaturewas refluxed for 2 hours
  2. extractionextracted with ethyl acetate
  3. washAfter the ethyl acetate layer was washed successively with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe residue obtained by evaporation of the solvent under reduced pressure
  6. customwas crystallized by dichloromethane/n-hexane

출처 및 근거

ORD 기록
ord-25a823ac4892465284d53ac0aeadec24
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07626042B2

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