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

HRID 1284552
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HRID 1284552 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b0e828e64f3647f58539f85402a7bedf
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04563477

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