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Ammonium formate → HCID 178491270、化合物

HRID 631868
ノート
印刷プレビュー

反応式

HRID 631868 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 68296418HCID 68296418、化合物2 回

生成物 1

HCID 178491270HCID 178491270、化合物収率 61.2%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ccad89960a8445c1984729ffe298fdba
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321740B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート