Ammonium formate → HCID 66736111、化合物

HRID 1640966ノート

反応式

HRID 1640966 の反応式
[C:1]1([S:7]([C:10]2[CH:11]=[CH:12][C:13]([N+:19]([O-])=O)=[C:14]([CH:18]=2)[C:15]([NH2:17])=[O:16])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])=O.[NH4+]>C(O)C.O.[Pd]>[NH2:19][C:13]1[CH:12]=[CH:11][C:10]([S:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)(=[O:9])=[O:8])=[CH:18][C:14]=1[C:15]([NH2:17])=[O:16]

参加物

6

反応物 2

HCID 2723923Ammonium formateHCID 66735912HCID 66735912、化合物

生成物 1

HCID 66736111HCID 66736111、化合物収率 66%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

5-Benzenesulfonyl-2-nitro-benzamide (3.13 g, 10.23 mmol) was suspended in absolute ethanol (200 mL), treated with 10% Pd/C (1.5 g) and then with ammonium formate (9.7 g, 153 mmol). The mixture was stirred at reflux. After a couple of hours the reaction was complete. After cooling to room temperature the reaction was filtered over celite and the panel was washed with EtOH. Evaporation of the filtrate left the crude product that was taken up with a small amount of methanol and added dropwise to 400 mL of iced water kept under stirring. The solid thus formed was filtered and washed with water affording 1.87 g of title compound (66% yield).

後処理

  1. temperatureat reflux
  2. waitAfter a couple of hours the reaction was complete
  3. filtrationwas filtered over celite
  4. washthe panel was washed with EtOH
  5. customEvaporation of the filtrate
  6. waitleft the crude product that
  7. additionadded dropwise to 400 mL of iced water
  8. stirringunder stirring
  9. customThe solid thus formed
  10. filtrationwas filtered

出典と根拠

ORDレコード
ord-1a8d5d4fe56146ceb40e1183caa9035b
出典データセット
uspto-grants-2012_02
特許番号
US08114865B2

反応ノート

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