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Pyromellitic dianhydride → HCID 10128976, 화합물

HRID 2307720
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HRID 2307720 반응식
[N:1]1[CH:6]=[CH:5][C:4]([O:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[CH2:11][NH:12][C@@H:13]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:16][CH2:15][CH2:14]2)=[CH:3][CH:2]=1.C(N(C(C)C)CC)(C)C.[CH:35]1[C:40]2[C:41]([O:43][C:44](=[O:45])[C:39]=2[CH:38]=[C:37]2[C:46]([O:48][C:49](=[O:50])[C:36]=12)=[O:47])=[O:42].C([O-])([O-])=[O:52].[Na+].[Na+]>C1COCC1>[N:1]1[CH:2]=[CH:3][C:4]([O:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[CH2:11][N:12]([C@@H:13]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:16][CH2:15][CH2:14]2)[C:41]([C:40]2[CH:35]=[C:36]([C:49]([OH:48])=[O:50])[C:37]([C:46]([OH:52])=[O:47])=[CH:38][C:39]=2[C:44]([OH:43])=[O:45])=[O:42])=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6966Pyromellitic dianhydrideHCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 69721082HCID 69721082, 화합물

생성물 1

HCID 10128976HCID 10128976, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The product from Example 106A (1.17 g), diisopropylethyl amine (2.5 mL, 14.4 mmol) and 1,2,4,5-benzenetetracarboxylic dianhydride (0.78 g, 3.58 mmol) in THF (30 mL) were processed as described in Example 1B. The reaction mixture was treated with saturated Na2CO3 solution (30 mL), and stirred vigorously at room temperature for 1 hour. The layers were separated and the aqueous layer was acidified with 1N HCl. The acidified aqueous layer was evaporated under reduced pressure to afford off-white plates. Soxhlet extraction (ethanol) of the crude solid, followed by RP-HPLC, provided the title compound (20 mg).

후처리

  1. customThe layers were separated
  2. customThe acidified aqueous layer was evaporated under reduced pressure
  3. customto afford off-white plates
  4. extractionSoxhlet extraction (ethanol) of the crude solid

출처 및 근거

ORD 기록
ord-af4788b417bf493980a035f5af43e3ca
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831193B2

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