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Sodium Hydroxide → 2-(4-Methoxy-benzoylamino)-pent-4-enoic acid

HRID 479140
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반응식

HRID 479140 반응식
C([O:3][C:4](=[O:20])[CH:5]([NH:9][C:10](=[O:19])[C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)[CH2:6][CH:7]=[CH2:8])C.[OH-].[Na+]>C1COCC1.CCO>[CH3:18][O:17][C:14]1[CH:13]=[CH:12][C:11]([C:10]([NH:9][CH:5]([CH2:6][CH:7]=[CH2:8])[C:4]([OH:20])=[O:3])=[O:19])=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 695565842-(4-Methoxy-benzoylamino)-pent-4-enoic acid ethyl ester

생성물 1

HCID 180035572-(4-Methoxy-benzoylamino)-pent-4-enoic acid

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

10.56 g of the above prepared 2-(4-methoxy-benzoylamino)-pent-4-enoic acid ethyl ester (38.1 mmol) was dissolved in 120 ml of THF/EtOH=1/1 and treated at 0° with 38 ml of 2N NaOH. The reaction mixture was kept at this temperature for 3 h. It was then poured onto crashed ice/HCl, extracted twice with AcOEt, washed with brine, and dried over natrium sulfate. Evaporation of the solvents, followed by crystallisation from AcOEt at −20°, yielded 8.41 g of the title acid as white crystals of m.p. 121-124°.

후처리

  1. additionIt was then poured
  2. extractionextracted twice with AcOEt
  3. washwashed with brine
  4. dry with materialdried over natrium sulfate
  5. customEvaporation of the solvents
  6. customfollowed by crystallisation from AcOEt at −20°
  7. customyielded 8.41 g of the title acid as white crystals of m.p. 121-124°

출처 및 근거

ORD 기록
ord-c1378c4b521643cfbd65089ab9f25ad2
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06642389B2

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