ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Phenol → Urea Urethane

HRID 1158185
ノート
印刷プレビュー

反応式

HRID 1158185 の反応式
CC1C=CC([N:8]=[C:9]=[O:10])=CC=1[N:11]=[C:12]=[O:13].C1C([NH2:20])=CC=C(S(C2C=CC(N)=CC=2)(=O)=O)C=1.[C:31]1([OH:37])C=CC=C[CH:32]=1.C(N(CC)CC)C>C(C(C)=O)C>[NH2:20][C:12]([NH2:11])=[O:13].[NH2:8][C:9]([O:37][CH2:31][CH3:32])=[O:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 996PhenolHCID 2955DapsoneHCID 8471TriethylamineHCID 11443Toluene 2,4-Diisocyanate

生成物 1

HCID 21585015Urea Urethane収率 549.8%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒4 回

反応条件

温度
30 °C

実験手順

To 158.5 g of 2,4-toluene diisocyanate was added 240 g of methyl ethyl ketone as a solvent, and 107.5 g of 4,4′-diaminodiphenyl sulfone was added thereto in the form of powder at 30° C. with stirring at 400 rpm over a period of 8 hours. After 1 hour, 26 g of methyl ethyl ketone was added thereto and stirred for another 15 hours to obtain a white viscous slurry reaction mixture. Then, a solution of 89.5 g of phenol in 15.8 g of methyl ethyl ketone was poured into the reaction mixture to be dissolved therein, after which 9.3 g of a 1 wt % solution of triethylamine in methyl ethyl ketone was added thereto as a catalyst over a period of 2 hours, and the reaction was uninterruptedly carried out for 1 hour. Thereafter, the reaction mixture was cooled to 20° C. and continuously stirred for 3 hours to obtain a slurry containing slightly yellow crystals precipitated therein. The slurry was freed of the solvent and concentrated under reduced pressure to be solidified, after which the resulting solid was ground and then dried overnight in a vacuum to obtain 355 g of a urea-urethane composition as slightly yellow powder.

後処理

  1. waitAfter 1 hour
  2. stirringstirred for another 15 hours
  3. customto obtain
  4. customa white viscous slurry reaction mixture
  5. dissolutionto be dissolved
  6. waitas a catalyst over a period of 2 hours
  7. waitthe reaction was uninterruptedly carried out for 1 hour
  8. temperatureThereafter, the reaction mixture was cooled to 20° C.
  9. stirringcontinuously stirred for 3 hours
  10. customto obtain a slurry
  11. additioncontaining slightly yellow crystals
  12. customprecipitated
  13. concentrationconcentrated under reduced pressure
  14. customdried overnight in a vacuum

出典と根拠

ORDレコード
ord-960d7d6d22e34aa193fc969503faf89e
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807738B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート