Water → HCID 12387514, 화합물

HRID 2367862노트

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HRID 2367862 반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][C:10]([CH3:19])([C:12](=[O:18])[CH2:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH3:11].C([O-])(=O)C.[NH4+].O>CC(C)(C)C#N>[Br:1][CH:13]([C:14]([CH3:17])([CH3:16])[CH3:15])[C:12](=[O:18])[C:10]([CH3:19])([CH3:9])[CH3:11]

참가 물질

6

반응물 4

HCID 962WaterHCID 67184N-bromobutanimide2회HCID 1366702,2,5,5-Tetramethyl-3-hexanoneHCID 517165Ammonium Acetate2회

생성물 1

HCID 12387514HCID 12387514, 화합물

시약·촉매·용매 1

HCID 12416Pivalonitrile용매

실험 절차

24 g of N-bromosuccinimide (0.1344 mol) was added to 10 g of 2,2,5,5-Tetramethyl-3-hexanone (0.064 mol) in 50 mL of trimethylacetonitrile. To this mixture, 10 g of ammonium acetate (0.1344 mol) was added within 5 minutes. This mixture was refluxed overnight then filtered. To the filtrate, 24 g of N-bromosuccinimide (0.1344 mol) and 10 g of ammonium acetate (0.1344 mol) was added, then refluxed for 5 hours. The reaction mixture was then cooled, 600 mL of water added, and the resulting mixture then filtered. The aqueous layer was washed three times with 50 ml of hexanes. The hexane fractions were then combined, washed three times with 50 ml of with water, then dried with anhydrous magnesium sulfate. Product was collected by distilling off the hexane at atmospheric pressure.

후처리

  1. temperatureThis mixture was refluxed overnight
  2. filtrationthen filtered
  3. temperaturerefluxed for 5 hours
  4. temperatureThe reaction mixture was then cooled
  5. filtrationthe resulting mixture then filtered
  6. washThe aqueous layer was washed three times with 50 ml of hexanes
  7. washwashed three times with 50 ml of with water
  8. dry with materialdried with anhydrous magnesium sulfate
  9. customProduct was collected
  10. distillationby distilling off the hexane at atmospheric pressure

출처 및 근거

ORD 기록
ord-4e5e363dbe2647739e1238344514c04d
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703103B2

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