Potassium Carbonate → HCID 88426431、化合物

HRID 465988ノート

反応式

HRID 465988 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 88426431HCID 88426431、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-718d871338834745b711958b6d497b62
出典データセット
uspto-grants-1992_10
特許番号
US05155121

反応ノート

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