Ammonium Acetate → HCID 68677556、化合物

HRID 2233016ノート

反応式

HRID 2233016 の反応式
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]

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 68675630HCID 68675630、化合物

生成物 1

HCID 68677556HCID 68677556、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-256a1cf901e64a268c09b48ce576c220
出典データセット
uspto-grants-2010_05
特許番号
US07709473B2

反応ノート

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