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Pyromellitic dianhydride → HCID 69721180, 화합물

HRID 2307722
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HRID 2307722 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][C:8]1[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=1)[CH2:11][NH:12][C@@H:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16][CH2:15][CH2:14]1.[CH:26]1[C:31]2[C:32]([O:34][C:35](=[O:36])[C:30]=2[CH:29]=[C:28]2[C:37]([O:39][C:40](=[O:41])[C:27]=12)=[O:38])=[O:33].C(N(C(C)C)CC)(C)C.C([O-])([O-])=[O:52].[Na+].[Na+]>>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[O:7][C:8]1[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=1)[CH2:11][N:12]([C@@H:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16][CH2:15][CH2:14]1)[C:32]([C:31]1[CH:26]=[C:27]([C:40]([OH:39])=[O:41])[C:28]([C:37]([OH:52])=[O:38])=[CH:29][C:30]=1[C:35]([OH:34])=[O:36])=[O:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6966Pyromellitic dianhydrideHCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 69720977HCID 69720977, 화합물

생성물 1

HCID 69721180HCID 69721180, 화합물

실험 절차

The product from Example 107A, 1,2,4,5-benzenetetracarboxylic dianhydride (0.125 g, 0.57 mmol) and diisopropylethyl amine (0.4 mL, 2.3 mmol) 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 a solid. Soxhlet extraction (ethanol) of the crude solid, followed by RP-HPLC, provided the title compound (4 mg).

후처리

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

출처 및 근거

ORD 기록
ord-d5658ca973514d6d92de6d7b0b8cfcce
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831193B2

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