Potassium Carbonate → HCID 88426431, 화합물

HRID 465988노트

반응식

HRID 465988 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)=O)[CH:2]=1.[Cl-].[OH:27][NH3+:28].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=[N:28][OH:27])[C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)[CH:2]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 21645Hydroxylamine HClHCID 149893984-Chloro-N-[3-(pyridine-3-carbonyl)phenyl]benzene-1-sulfonamide

생성물 1

HCID 88426431HCID 88426431, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

7.45 g (20 mmol) of the compound from Example 1, 2.08 g (30 mmol) of hydoxylammonium chloride and 4.14 g (30 mmol) of potassium carbonate are refluxed in 20 ml of ethanol for 15 h. After cooling to room temperature, the mixture is evaporated and the residue is stirred in 50 ml of water for 3 h (after this time no oily residues, but only crystalline residues, were still undissolved). The precipitate was filtered off, washed with water and recrystallised from methanol by addition of water. Yield: 5.71 g (73.7% of theory) M.p.: 170° C.

후처리

  1. customthe mixture is evaporated
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customrecrystallised from methanol by addition of water

출처 및 근거

ORD 기록
ord-718d871338834745b711958b6d497b62
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155121

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