Malonic Acid → HCID 86735523、化合物

HRID 1679084ノート

反応式

HRID 1679084 の反応式
[K:1].[S:2]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13]([NH2:15])=[O:14])=[CH:8][CH:7]=1)([OH:5])(=[O:4])=[O:3].[C:16](O)(=[O:21])[CH2:17][C:18](O)=[O:19].C(OC(=O)C)(=O)C>C(O)(=O)C>[S:2]([C:6]1[CH:7]=[CH:8][C:9]([N:12]2[C:16](=[O:21])[CH2:17][C:18](=[O:19])[NH:15][C:13]2=[O:14])=[CH:10][CH:11]=1)([OH:5])(=[O:4])=[O:3].[K:1]

参加物

5

反応物 3

HCID 867Malonic AcidHCID 7918Acetic Anhydride3 回HCID 8673552413846-15-6

生成物 1

HCID 86735523HCID 86735523、化合物収率 91.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
95 °C

実験手順

A mixture of 29.9 g of N-(4-sulfophenyl)urea potassium salt, 15 g of malonic acid and 200 ml of glacial acetic acid was heated to 60° to 70° C with stirring and 300 ml of acetic anhydride was added dropwise to the mixture. After about 50 ml of the acetic anhydride had been added, the mixture dissolved. After all of the acetic anhydride (300 ml) was added, the temperature of the reaction solution increased to 95° C. The reaction solution was stirred for 4 hours and then condensed under reduced pressure so as to precipitate crystals. 700 ml of ethanol was added to the condensed solution and the crystals were completely precipitated. The precipitated crystals were collected by filtration, washed thoroughly with ethanol and dried by heating under reduced pressure to obtain 34.5 g of crystals. The obtained crystals were recrystallized using a 90% methanol aqueous solution and, thereby, 29.3 g of white crystals was obtained. Melting point: above 300° C. Elemental Analysis:

後処理

  1. temperaturewas heated to 60° to 70° C
  2. dissolutionthe mixture dissolved
  3. stirringThe reaction solution was stirred for 4 hours
  4. customcondensed under reduced pressure so as
  5. customto precipitate crystals
  6. addition700 ml of ethanol was added to the condensed solution
  7. customthe crystals were completely precipitated
  8. filtrationThe precipitated crystals were collected by filtration
  9. washwashed thoroughly with ethanol
  10. customdried
  11. temperatureby heating under reduced pressure

出典と根拠

ORDレコード
ord-41808a84371148b6a759cc22bdeda7a9
出典データセット
uspto-grants-1978_03
特許番号
US04078933

反応ノート

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