Hydrogen Sulfide → 3-Mercaptopyridine-2-sulfonamide

HRID 1655068

反応式

HRID 1655068 の反応式
[SH2:1].CC([O-])(C)C.[K+].F[C:9]1[C:10]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:11][CH:12]=[CH:13][CH:14]=1>CN(C)C=O>[SH:1][C:9]1[C:10]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:11][CH:12]=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 402Hydrogen Sulfide2 回HCID 199579303-Fluoropyridine-2-sulfonamideHCID 23665647Potassium tert-butoxide2 回

生成物 1

HCID 1274273-Mercaptopyridine-2-sulfonamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.06 g of hydrogen sulfide are passed at a temperature of +16° to +20° C. under a nitrogen atmosphere into a mixture of 6.88 g of potassium tert-butylate and 5 g of 3-fluoropyridin-2-ylsulfonamide in 90 ml of dimethylformamide. After the mixture has been stirred for 41/2 hours at a temperature of +50° C., 0.32 g of potassium tert-butylate are added and 0.1 g of hydrogen sulfide is passed in. After the reaction mixture has been stirred for 2 hours at a temperature of +50° C., it is concentrated in vacuo at a temperature of +75° C. The resulting oily residue is triturated with 135 ml of cold 0.75N sulfuric acid. After the residue has been filtered and washed with a little water, the resulting product is dried in vacuo over phosphorus pentoxide. This gives 3.58 g of 3-mercaptopyridin-2-ylsulfonamide of a melting point of +102° to +104° C.

後処理

  1. additionare added
  2. concentrationis concentrated in vacuo at a temperature of +75° C
  3. customThe resulting oily residue is triturated with 135 ml of cold 0.75N sulfuric acid
  4. filtrationAfter the residue has been filtered
  5. washwashed with a little water
  6. dry with materialthe resulting product is dried in vacuo over phosphorus pentoxide

出典と根拠

ORDレコード
ord-efc3701ebb034da199312f16b9974500
出典データセット
uspto-grants-1995_04
特許番号
US05410063

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