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3-Nitrophthalic anhydride → HCID 22241217, 화합물

HRID 989785
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HRID 989785 반응식
[O:1]=[C:2]1[CH:7]([NH:8][C:9]([O:11]CC2C=CC=CC=2)=O)[CH2:6][CH:5]([O:19][C:20](=[O:22])[CH3:21])[C:4](=[O:23])[NH:3]1.[N+:24]([C:27]1[CH:37]=[CH:36][CH:35]=[C:29]2C([O:32][C:33](=O)[C:28]=12)=O)([O-:26])=[O:25]>C(O)(=O)C.[Pd]>[N+:24]([C:27]1[CH:37]=[CH:36][CH:35]=[C:29]2[C:28]=1[C:33](=[O:32])[N:8]([CH:7]1[CH2:6][CH:5]([O:19][C:20](=[O:22])[CH3:21])[C:4](=[O:23])[NH:3][C:2]1=[O:1])[C:9]2=[O:11])([O-:26])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 216313-Nitrophthalic anhydrideHCID 12047333HCID 12047333, 화합물

생성물 1

HCID 22241217HCID 22241217, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

A solution of 2,6-dioxo-3-benzyloxycarbonylamino-5-acetoxypiperidine (9 g, 28.2 mmol) and Pd/C (10%, 0.9 g) in acetic acid (90 mL) is shaken under hydrogen (50-60 psi) for 3 hours. The suspension is filtered through a pad of Celite and washed with acetic acid. To the filtrate is added 3-nitrophthalic anhydride (5.4 g, 28.2 mmol), this mixture is heated at reflux for 18 hours, and the solvent is then removed in vacuo to give 3-(4-nitro-1,3-dioxoisoindolin-2-yl)-2,6-dioxo-5-acetoxypiperidine which can be further purified by column chromatography.

후처리

  1. filtrationThe suspension is filtered through a pad of Celite
  2. washwashed with acetic acid
  3. temperaturethis mixture is heated
  4. temperatureat reflux for 18 hours
  5. customthe solvent is then removed in vacuo

출처 및 근거

ORD 기록
ord-fe8a5e4614e1400fa16e2e163a1bfa41
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458810B1

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