Salicyloyl chloride → HCID 70563405、化合物

HRID 435955

反応式

HRID 435955 の反応式
C(O[C:5]1[N:10]=[C:9](NN)[N:8]=[C:7]([NH:13][NH2:14])[N:6]=1)CC.[C:15](Cl)(=[O:23])[C:16]1[C:17](=[CH:19][CH:20]=[CH:21][CH:22]=1)[OH:18]>CC(N(C)C)=O>[CH2:17]([O:18][NH:14][NH:13][C:7]1[N:6]=[C:5]([C:15](=[O:23])[C:16]2[C:17](=[CH:19][CH:20]=[CH:21][CH:22]=2)[OH:18])[N:10]=[C:9]([C:15](=[O:23])[C:16]2[C:17](=[CH:19][CH:20]=[CH:21][CH:22]=2)[OH:18])[N:8]=1)[CH2:16][CH3:15]

参加物

4

反応物 2

HCID 74041Salicyloyl chlorideHCID 214549262-Propoxy-4,6-dihydrazino-s-triazine

生成物 1

HCID 70563405HCID 70563405、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

20 g of 2-propoxy-4,6-dihydrazino-s-triazine (melting point 130° C) are dissolved in 200 ml of dimethylacetamide and treated with 32 g of salicyloyl chloride at 10° - 20°, over the course of 30 minutes, whilst stirring and cooling externally. The reaction is exothermic. The homogeneous reaction mixture is stirred for a further 30 minutes at 20° C and is subsequently clarified by filtration and slowly treated with 500 ml of water whilst stirring, whereupon the reaction product precipitates as a white solid. The precipitate is filtered of, washed with water, dried at 80° C and purified by recrystallisation from dioxane. The 2-propoxy-4,6-disalicyloylhydrazino-s-triazine obtained (Stabiliser No. 4) has a melting point of 258°-260° C.

後処理

  1. temperaturecooling externally
  2. stirringThe homogeneous reaction mixture is stirred for a further 30 minutes at 20° C
  3. filtrationis subsequently clarified by filtration
  4. additionslowly treated with 500 ml of water
  5. stirringwhilst stirring, whereupon the reaction product
  6. customprecipitates as a white solid
  7. filtrationThe precipitate is filtered of,
  8. washwashed with water
  9. customdried at 80° C
  10. custompurified by recrystallisation from dioxane

出典と根拠

ORDレコード
ord-bc0fdbd4fc8d4da380012c5f0a4a23f1
出典データセット
uspto-grants-1977_02
特許番号
US04007183

関連ノート

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