Hydrochloric Acid → 4-(Hydrazinocarbonyl)benzoic acid

HRID 973537

反応式

HRID 973537 の反応式
[C:1]([O:12]C)(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([O-])=[O:7])=[CH:4][CH:3]=1.O.[NH2:15][NH2:16].Cl>CO>[C:1]([C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH:15][NH2:16])=[O:7])=[CH:4][CH:3]=1)([OH:12])=[O:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 36144541,4-Benzenedicarboxylic acid, methyl ester

生成物 1

HCID 2794374-(Hydrazinocarbonyl)benzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 1 l of methanol was dissolved 180 g of monomethyl terephthalate, and the solution was slowly added dropwise to 500 ml of hydrazine hydrate (50%) at room temperature while stirring. After the drop-wise addition, the mixture was heat-refluxed for 5 hours while stirring. A hydrochloric acid aqueous solution was slowly added to the reaction mixture to adjust to a pH of about 1 to thereby precipitate white crystals. Two liters of water was added to the system, followed by stirring for a while. The formed crystals were collected by filtration under reduced pressure, washed twice with 200 ml of water, and dried to obtain 160 g of p-carboxybenzhydrazide (melting point: 235-236° C.).

後処理

  1. additionAfter the drop-wise addition
  2. temperaturethe mixture was heat-refluxed for 5 hours
  3. stirringwhile stirring
  4. customto thereby precipitate white crystals
  5. additionTwo liters of water was added to the system
  6. stirringby stirring for a while
  7. filtrationThe formed crystals were collected by filtration under reduced pressure
  8. washwashed twice with 200 ml of water
  9. customdried

出典と根拠

ORDレコード
ord-fdb0439c7795491b846d322bb06d0045
出典データセット
uspto-grants-1991_11
特許番号
US05064751

関連ノート

読み込み中…