Ammonium formate → HCID 66736111, 화합물

HRID 1640966노트

반응식

HRID 1640966 반응식
[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]

참가 물질

6

반응물 2

HCID 2723923Ammonium formateHCID 66735912HCID 66735912, 화합물

생성물 1

HCID 66736111HCID 66736111, 화합물수율 66%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1a8d5d4fe56146ceb40e1183caa9035b
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114865B2

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