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Tetrahydrofuran → HCID 15980985, 화합물

HRID 1692170
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HRID 1692170 반응식
[CH3:1][O:2][C:3](=[CH:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=1)[C:4]([OH:6])=[O:5].C1COCC1>CO.[Pd]>[CH3:1][O:2][CH:3]([CH2:7][C:8]1[CH:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=1)[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8028TetrahydrofuranHCID 669056512-Methoxy-3-(4-nitrophenyl)prop-2-enoic acid

생성물 1

HCID 15980985HCID 15980985, 화합물수율 88%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

2-Methoxy-3-(4-nitrophenyl)acrylic acid (6.7 g, 30 mmol) was taken up in methanol (700 ml) and THF (300 ml) and 10% Pd on C (wet basis) (0.67 g) was added. The mixture was hydrogenated at 45 psi for 43 mins, followed by repeated refills to 45-48 psi every hour for 3 hr and finally 48 psi for 18 hr. The resulting suspension was filtered through GF/F filter paper and the filter residue washed with MeOH (200 ml). The filtrates were concentrated to an off-white solid. The solid was slurried in IMS (75 ml) at 20° C. for 1.5 hr, filtered, and washed with IMS/heptane (1:2) (20 ml) and dried on the filter for 1 hr to afford (±)-2-methoxy-3-(4′-aminophenyl)-propionic acid as an off-white solid (5.1 g, 88% yield)

후처리

  1. customfor 3 hr
  2. waitfinally 48 psi for 18 hr
  3. filtrationThe resulting suspension was filtered through GF/F
  4. filtrationfilter paper
  5. washthe filter residue washed with MeOH (200 ml)
  6. concentrationThe filtrates were concentrated to an off-white solid
  7. waitThe solid was slurried in IMS (75 ml) at 20° C. for 1.5 hr
  8. filtrationfiltered
  9. washwashed with IMS/heptane (1:2) (20 ml)
  10. customdried on the
  11. filtrationfilter for 1 hr

출처 및 근거

ORD 기록
ord-ad4051d9656b41048b1f6f56a84cf5d7
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153841B2

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