Water → 2-Hydroxybenzoic acid 2-(2-hydroxybenzoyl)hydrazide

HRID 1730615

反応式

HRID 1730615 の反応式
[C:1]([NH:10][NH2:11])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[C:12](Cl)(=[O:20])[C:13]1[C:14](=[CH:16][CH:17]=[CH:18][CH:19]=1)[OH:15].O>CC(N(C)C)=O>[C:1]([NH:10][NH:11][C:12](=[O:20])[C:13]1[C:14](=[CH:16][CH:17]=[CH:18][CH:19]=1)[OH:15])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4]

参加物

5

反応物 3

HCID 962WaterHCID 13637Salicylic acid, hydrazideHCID 74041Salicyloyl chloride

生成物 1

HCID 653032-Hydroxybenzoic acid 2-(2-hydroxybenzoyl)hydrazide

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

30.4 g of salicylic acid hydrazide are dissolved in 500 ml of dimethylacetamide and 34.8 g of salicylic acid chloride are added dropwise over the course of 70 minutes at 25° - 40° C. The yellow solution is stirred for 3 hours at room temperature and is then poured into 1 liter of water, whereupon white, fine crystals precipitate. The substance is filtered off, washed with water and dried in vacuo at 60° C. The product is purified by recrystallisation from ethylene gylcol monomethyl ether. The N,N'-bis-salicyloyl-hydrazine thus obtained (stabiliser No. 1), melts at 303° C.

後処理

  1. filtrationThe substance is filtered off
  2. washwashed with water
  3. customdried in vacuo at 60° C
  4. customThe product is purified by recrystallisation from ethylene gylcol monomethyl ether

出典と根拠

ORDレコード
ord-95adfce7284f4d9991794887c78487ea
出典データセット
uspto-grants-1976_11
特許番号
US03993622

関連ノート

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