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Ammonium Acetate → HCID 178513844, 화합물

HRID 1463230
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HRID 1463230 반응식
[F:1][C:2]1[N:7]=[C:6]2[NH:8][N:9]=[C:10]([C:11]([O:13]C(C)(C)C)=O)[C:5]2=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+:22]>FC(F)(F)C(O)=O>[F:1][C:2]1[N:7]=[C:6]2[NH:8][N:9]=[C:10]([C:11]([NH2:22])=[O:13])[C:5]2=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 178450870HCID 178450870, 화합물

생성물 1

HCID 178513844HCID 178513844, 화합물수율 89.1%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

t-Butyl 6-fluoro-1H-pyrazolo[3,4-b]pyridine-3-carboxylate (8.90 g, 37.5 mmole) was dissolved in 30 mL of trifluoroacetic acid and allowed to stand undisturbed for 2 hours. The solvent was then evaporated and the residue was dissolved in 30 mL of DMF. N,N'-Carbonyldiimidazole (7.0 g, 43.2 mmol) was added and the reaction mixture was stirred overnight. Ammonium acetate (8.7 g, 113 mmol) was then added to the resulting suspendion and stirring was continued for 4 hours. The solvent was evaporated under high vacuum and the residue was triturated well with H2O to give 6.02 g (89%) of product after drying. An analytical sample was obtained by recrystallization from HOAc, mp 295° C. (dec).

후처리

  1. customThe solvent was then evaporated
  2. dissolutionthe residue was dissolved in 30 mL of DMF
  3. stirringstirring
  4. waitwas continued for 4 hours
  5. customThe solvent was evaporated under high vacuum
  6. customthe residue was triturated well with H2O

출처 및 근거

ORD 기록
ord-600a837bffa34c74a0c4966c53af5ea1
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05300498

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