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4-(2-Nitrophenyl)-2-phthalimidobutyric acid → 4-(2-Aminophenyl)-2-phthalimidobutyric acid

HRID 2351225
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반응식

HRID 2351225 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][CH2:11][CH:12]([N:16]1[C:20](=[O:21])[C:19]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:18]2[C:17]1=[O:26])[C:13]([OH:15])=[O:14])([O-])=O>CO.[C].[Pd]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][CH2:11][CH:12]([N:16]1[C:20](=[O:21])[C:19]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:18]2[C:17]1=[O:26])[C:13]([OH:15])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 144072514-(2-Nitrophenyl)-2-phthalimidobutyric acid

생성물 1

HCID 140106814-(2-Aminophenyl)-2-phthalimidobutyric acid수율 84.9%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

In 300 ml of methanol, 13 g of 4-(2-nitrophenyl)-2-phthalimidobutyric acid is catalytically reduced at ambient temperature and under atmospheric pressure with use of 3 g of 5% palladium-carbon as a catalyst. After the calculated amount of hydrogen is absorbed, the insoluble material is separated by filtration, and washed four times with 300 ml of acetone. The acetone washings and the methanol portion are combined and concentrated under reduced pressure. The residue is admixed with 50 ml of ethanol, and the crystals which separate out are collected by filtration to give 10.1 g of 4-(2-aminophenyl)-2-phthalimidobutyric acid as yellow prisms. m.p. 198°-203° C. (decomp.).

후처리

  1. customAfter the calculated amount of hydrogen is absorbed
  2. customthe insoluble material is separated by filtration
  3. washwashed four times with 300 ml of acetone
  4. concentrationconcentrated under reduced pressure
  5. customthe crystals which separate out
  6. filtrationare collected by filtration

출처 및 근거

ORD 기록
ord-b44662a576d242629dc4e7ee963a3805
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04871842

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