3-(N-carbethoxymethyl-N-methylsulfamoyl)-thiophene-2-carboxylic acid methyl ester → 2H-Thieno(2,3-e)-1,2-thiazine-3-carboxylic acid, 4-hydroxy-2-methyl-, methyl ester, 1,1-dioxide

HRID 616825

反応式

HRID 616825 の反応式
C[O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[S:10](=[O:20])(=[O:19])[N:11]([CH2:13][C:14]([O:16][CH2:17]C)=[O:15])[CH3:12])=O.C[O-].[Na+]>>[C:14]([C:13]1[N:11]([CH3:12])[S:10](=[O:20])(=[O:19])[C:9]2[CH:8]=[CH:7][S:6][C:5]=2[C:3]=1[OH:2])([O:16][CH3:17])=[O:15]

参加物

3

反応物 2

HCID 28087943-(N-carbethoxymethyl-N-methylsulfamoyl)-thiophene-2-carboxylic acid methyl esterHCID 10942334Sodium Methoxide

生成物 1

HCID 546905992H-Thieno(2,3-e)-1,2-thiazine-3-carboxylic acid, 4-hydroxy-2-methyl-, methyl ester, 1,1-dioxide

実験手順

13.2 G. of 3-(N-carbethoxymethyl-N-methyl-sulfamoyl)-thiophene-2-carboxylic acid methyl ester are suspended in 42 ml. of a 1-N methanolic sodium methylate solution in the cold and under a nitrogen stream. After stirring for 15 minutes, a clear solution results. The solution is heated to reflux for 20 minutes, then cooled, neutralized and evaporated in vacuo. The residue is taken up in methylene chloride, shaken once each time with water and a sodium bicarbonate solution, dried and evaporated. The residue is brought to crystallization with methanol. There is obtained 3-carbomethoxy-4-hydroxy-2-methyl-2H-thieno[2,3-e]-1,2-thiazine1,1-dioxide of melting point 193°-195° C.

後処理

  1. customa clear solution results
  2. temperatureThe solution is heated
  3. temperatureto reflux for 20 minutes
  4. temperaturecooled
  5. customevaporated in vacuo
  6. stirringshaken once each time with water
  7. dry with materiala sodium bicarbonate solution, dried
  8. customevaporated
  9. customThe residue is brought to crystallization with methanol

出典と根拠

ORDレコード
ord-f2f22dc75bbd48ba9cece738d623e190
出典データセット
uspto-grants-1978_02
特許番号
US04076709

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