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Ammonium formate → HCID 178491270, 화합물

HRID 631868
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HRID 631868 반응식
C([N:8]1[C:12]([C:13]2[C:18]([O:19][CH3:20])=[CH:17][CH:16]=[CH:15][C:14]=2[NH:21][S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)(=[O:24])=[O:23])=[N:11][N:10]=[N:9]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>C(O)C.[OH-].[Pd+2].[OH-]>[CH3:20][O:19][C:18]1[C:13]([C:12]2[NH:8][N:9]=[N:10][N:11]=2)=[C:14]([NH:21][S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)(=[O:24])=[O:23])[CH:15]=[CH:16][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 68296418HCID 68296418, 화합물2회

생성물 1

HCID 178491270HCID 178491270, 화합물수율 61.2%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

실험 절차

A mixture of N-[2-(1-benzyl-1H-tetrazol-5-yl)-3-methoxyphenyl]-benzenesulfonamide (Intermediate 12, 0.104 g), ammonium formate (0.45 g) and palladium hydroxide (0.01 g) in ethanol (10 mL) was heated at reflux for 72 hours. The reaction mixture was filtered through celite and the filtrate was evaporated under vacuum. The residue was purified by flash chromatography on silica, eluting with a mixture of DCM and methanol. The fractions containing the desired product were combined and evaporated to give the title compound as a colorless solid (0.05 g).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 72 hours
  3. filtrationThe reaction mixture was filtered through celite
  4. customthe filtrate was evaporated under vacuum
  5. customThe residue was purified by flash chromatography on silica
  6. washeluting with a mixture of DCM and methanol
  7. additionThe fractions containing the desired product
  8. customevaporated

출처 및 근거

ORD 기록
ord-ccad89960a8445c1984729ffe298fdba
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321740B2

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