Phenol → 1,4-Bis(1,3,4-oxadiazolin-5-one-2-yl) butane

HRID 1005433ノート

反応式

HRID 1005433 の反応式
[C:1](Cl)(Cl)=[O:2].[C:5]([NH:15][NH2:16])(=[O:14])[CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][NH2:13])=[O:11].[C:17]1([OH:23])C=CC=CC=1>>[O:11]1[C:17](=[O:23])[NH:13][N:12]=[C:10]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1[O:14][C:1](=[O:2])[NH:16][N:15]=1

参加物

4

反応物 3

HCID 996PhenolHCID 6371Phosgene2 回HCID 66117Adipic Dihydrazide

生成物 1

HCID 154110221,4-Bis(1,3,4-oxadiazolin-5-one-2-yl) butane

反応条件

温度
85 °C

実験手順

A solution of 200 g of phosgene in 1.6 kg of phenol was introduced at 20° C. into a 4-liter phosgenation apparatus, and 174 g of adipic acid dihydrazide were added thereto. The mixture was heated to 85° C. within one hour, with stirring; gas evolved above a reaction temperature of 45° C. Phosgene was then introduced into the reaction mixture at 85° C. over 5 hours (approx. 30 g per hour), with stirring. The solution was then purged with nitrogen at 85 to 90° C. for 30 minutes, and the major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C. The remaining product was dissolved in 1 liter of toluene at 60° C. and precipitated by cooling to 20° C. The precipitate was suction filtered, washed with toluene and dried under vacuum.

後処理

  1. additionwere added
  2. customevolved above a reaction temperature of 45° C
  3. stirringwith stirring
  4. customThe solution was then purged with nitrogen at 85 to 90° C. for 30 minutes
  5. customthe major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C
  6. dissolutionThe remaining product was dissolved in 1 liter of toluene at 60° C.
  7. customprecipitated
  8. temperatureby cooling to 20° C
  9. filtrationfiltered
  10. washwashed with toluene
  11. customdried under vacuum

出典と根拠

ORDレコード
ord-eab9f2b47710408f940b8159016bfb8b
出典データセット
uspto-grants-2000_04
特許番号
US06054528

反応ノート

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