Ammonium Acetate → HCID 68677556, 화합물

HRID 2233016노트

반응식

HRID 2233016 반응식
C([O:3][C:4]([C:6]1[N:10]([CH2:11][C:12](=O)[C:13]([CH3:16])([CH3:15])[CH3:14])[C:9](=[O:18])[N:8]([C:19]([CH3:22])([CH3:21])[CH3:20])[N:7]=1)=O)C.C([O-])(=O)C.[NH4+:27]>CO>[C:19]([N:8]1[C:9](=[O:18])[N:10]2[CH:11]=[C:12]([C:13]([CH3:16])([CH3:15])[CH3:14])[NH:27][C:4](=[O:3])[C:6]2=[N:7]1)([CH3:22])([CH3:21])[CH3:20]

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 68675630HCID 68675630, 화합물

생성물 1

HCID 68677556HCID 68677556, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 8.60 g of the product of Step C and 21.30 g of ammonium acetate in MeOH was heated in a sealed system at 100° C. for 24 h. The solution was cooled to ambient temperature and concentrated to leave an oil that was partitioned between EtOAc and water. The aqueous layer was acidified to pH 5 with concentrated HCl and then extracted with EtOAc. The combined organic layers were washed with sat. sodium chloride, dried over sodium sulfate, filtered, and concentrated to provide 2,6-di-tert-butyl-2H,7H-[1,2,4]triazolo[4,3-a]pyrazine-3,8-dione as a white solid. MS (M+H+)=265.3.

후처리

  1. concentrationconcentrated
  2. customto leave an oil that
  3. customwas partitioned between EtOAc and water
  4. extractionextracted with EtOAc
  5. washThe combined organic layers were washed with sat. sodium chloride
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-256a1cf901e64a268c09b48ce576c220
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709473B2

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