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Sodium Hydroxide → HCID 12634259、化合物

HRID 1112718
ノート
印刷プレビュー

反応式

HRID 1112718 の反応式
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[C:15]([NH:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=O)[C:16]([CH3:19])([CH3:18])[CH3:17].[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:17][C:16]([C:15]1[O:24][C:23]([O:25][CH2:26][CH3:27])=[CH:22][N:21]=1)([CH3:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 3622015HCID 3622015、化合物

生成物 1

HCID 12634259HCID 12634259、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a vigorously-stirred slurry of phosphorus pentoxide (163.8 g., 1.15 mole) in chloroform (600 ml.) maintained under a nitrogen atmosphere is added slowly a solution of ethyl N-pivaloylglycinate (107.8 g., 0.576 mole) in chloroform (350 ml.). Upon completing the addition, the reaction mixture is stirred and heated at reflux under a nitrogen atmosphere for 14 hours. The cooled reaction mixture is treated with 20% sodium hydroxide (800 ml.), vigorously stirred for 1/2 hour and allowed to separate into two phases. After discarding the aqueous phase, the organic phase is washed with water and saturated brine, dried over sodium sulfate and filtered. Distillation of the filtrate provides 2-(1,1-dimethylethyl)-5-ethoxyoxazole as a pale yellow liquid (64 g., 66%), b.p. 58°-64° C./0.7 mm.

後処理

  1. additionthe addition
  2. temperatureheated
  3. temperatureat reflux under a nitrogen atmosphere for 14 hours
  4. customThe cooled reaction mixture
  5. stirringvigorously stirred for 1/2 hour
  6. customto separate into two phases
  7. washthe organic phase is washed with water and saturated brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. distillationDistillation of the filtrate

出典と根拠

ORDレコード
ord-6874b87b4c1e465aa354ef167fc98571
出典データセット
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04123537

反応ノート

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