Oxalic acid, dihydrazide → N,N'-bis-(salicyloyl)-oxalic acid dihydrazide

HRID 596753

反応式

HRID 596753 の反応式
[C:1]([NH:7][NH2:8])([C:3]([NH:5][NH2:6])=[O:4])=[O:2].[C:9](Cl)(=[O:17])[C:10]1[C:11](=[CH:13][CH:14]=[CH:15][CH:16]=1)[OH:12]>CC(N(C)C)=O>[C:9]([N:5]([C:3](=[O:4])[C:1]([NH:7][NH2:8])=[O:2])[NH:6][C:9](=[O:17])[C:10]1[C:11](=[CH:13][CH:14]=[CH:15][CH:16]=1)[OH:12])(=[O:17])[C:10]1[C:11](=[CH:13][CH:14]=[CH:15][CH:16]=1)[OH:12]

参加物

4

反応物 2

HCID 13826Oxalic acid, dihydrazideHCID 74041Salicyloyl chloride

生成物 1

HCID 21885000N,N'-bis-(salicyloyl)-oxalic acid dihydrazide

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
100 °C

実験手順

35.4 g of oxalic acid bis-hydrazide are suspended in 1000 ml of dimethyl acetamide, the suspension is briefly heated to 100° C and cooled to room temperature, and 93.5 g of salicylic acid chloride are slowly added in such a way that the reaction temperature does not exceed 40° C. After a further 15 minutes' stirring a largely homogeneous, yellowish solution has been obtained. After filtering off the undissolved constituents, the solution is mixed with 1.2 liters of ice water, whereupon the reaction product precipitates. The substance is filtered off, washed with water and purified by again precipitating it from dimethyl acetamide solution by means of water. After isolation and intensive drying at 130° C in vacuo, N,N'-bis-(salicyloyl)-oxalic acid dihydrazide (Stabiliser No. 2) is obtained as a white powder of melting point>320° C (decomposition).

後処理

  1. temperaturecooled to room temperature
  2. customdoes not exceed 40° C
  3. customhas been obtained
  4. filtrationAfter filtering off the undissolved constituents
  5. additionthe solution is mixed with 1.2 liters of ice water, whereupon the reaction product
  6. customprecipitates
  7. filtrationThe substance is filtered off
  8. washwashed with water
  9. custompurified
  10. customby again precipitating it from dimethyl acetamide solution by means of water
  11. customAfter isolation and intensive drying at 130° C in vacuo

出典と根拠

ORDレコード
ord-374ac00e3f1048baab367ca319eb87f8
出典データセット
uspto-grants-1977_03
特許番号
US04012360

関連ノート

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