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Methanesulfonic Acid → HCID 178492080, 화합물

HRID 1600028
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HRID 1600028 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:26])[C:7]3[C:14](=[O:15])[N:13]([NH:16][C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=4)[C:12](=[O:25])[C:8]=3[NH:9][C:10]=2[CH:11]=1.CS(O)(=O)=O>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:26])[C:7]3[C:14]([OH:15])=[N:13][N:16]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=4)[C:12](=[O:25])[C:8]=3[NH:9][C:10]=2[CH:11]=1
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참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 219976996-Chloro-2-(4-methoxyanilino)-2,3,4,9-tetrahydro-1H-pyrrolo[3,4-b]quinoline-1,3,9-trione

생성물 1

HCID 178492080HCID 178492080, 화합물수율 44%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6-Chloro-2-(4-methoxyanilino)-2,3,4,9-tetrahydro-1H-pyrrolo[3,4-b]-quinoline-1,3,9-trione (2.72 g, 7.40 mM was stirred in methanol (200 mL), and methanesulfonic acid (50 mL) was added. The tan suspension was heated to reflux for 16 hours during which it turned yellow. This yellow suspension was cooled to room temperature and filtered (the filtrate was saved for use in Example 8). The collected solids were washed with methanol to give the title compound as a yellow powder (1.19 g, 44%), mp 371°-373° C.; MS(CI): 370 (M+H). Analysis for C18 H2ClN3O4 : Calculated: C, 58.50; H, 3.27; N, 11.36; Found: C, 58.30; H, 3.41; N, 10.92; NMR: 13.33 (br s, 1H, exchangeable), 12.47 (s, 1H, exchangeable), 8.30 (d, J=8.73 Hz, 1H), 8.23 (br s, 1H), 7.61 (m, 3H), 7.08 (d, J=8.90 Hz, 2H), 3.83 (s, 3H).

후처리

  1. temperatureThe tan suspension was heated
  2. temperatureto reflux for 16 hours during which it
  3. filtrationfiltered (the filtrate
  4. washThe collected solids were washed with methanol

출처 및 근거

ORD 기록
ord-e45658ceb88e4059bf514bb4dbcf8071
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05744471

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