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N-Phenylglycine ethyl ester → ETHYL 2-PHENYL-2-(1H-PYRROL-1-YL)ACETATE

HRID 1284552
ノート
印刷プレビュー

反応式

HRID 1284552 の反応式
[C:1]1([NH:7][CH2:8][C:9](OCC)=O)[CH:6]=CC=CC=1.C(O[CH:17]1[CH2:21][CH2:20][CH:19]([O:22][CH2:23][CH3:24])[O:18]1)C>C(O)(=O)C>[N:7]1([CH:20]([C:21]2[CH:17]=[CH:17][CH:21]=[CH:20][CH:19]=2)[C:19]([O:22][CH2:23][CH3:24])=[O:18])[CH:1]=[CH:6][CH:9]=[CH:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 75190N-Phenylglycine ethyl esterHCID 955002,5-Diethoxytetrahydrofuran

生成物 1

HCID 2798193ETHYL 2-PHENYL-2-(1H-PYRROL-1-YL)ACETATE

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

52.8 g (0.24 mole) of ethyl phenylglycinate were dissolved in 136 ml of glacial acetic acid. Thereafter 39 g (0.24 mole) of 2,5-diethoxytetrahydrofuran were added over 10-15 minutes with stirring. The mixture was heated under reflux for one hour. After this time had elapsed, the mixture was allowed to cool and the major portion of the acetic acid was drawn off under reduced pressure. Finally, the residue was distilled under vacuum and the fraction distilling out at 115°-118° C. at 0.2 mm Hg was collected. The product obtained was first a colourless oil which crystallised on cooling, adopting a waxy aspect and weighing 46.5 g (70%). M.p. 51°-53° C. Centesimal composition: 73.31% C.; 6.08% N; 6.53% H. The IR spectrum in 0.5% KBr is illustrated in FIG. 1.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for one hour
  3. temperatureto cool
  4. distillationFinally, the residue was distilled under vacuum
  5. distillationthe fraction distilling out at 115°-118° C. at 0.2 mm Hg
  6. customwas collected
  7. customThe product obtained
  8. customcrystallised
  9. temperatureon cooling

出典と根拠

ORDレコード
ord-b0e828e64f3647f58539f85402a7bedf
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04563477

反応ノート

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