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Diethyl Ether → HCID 178515074, 화합물

HRID 323612
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HRID 323612 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:26])[C:7]3[C:15]([OH:16])=[N:14][N:13]([C:17]4[CH:22]=[CH:21][C:20]([O:23]C)=[CH:19][CH:18]=4)[C:12](=[O:25])[C:8]=3[NH:9][C:10]=2[CH:11]=1.C(OCC)C>CS(O)(=O)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:26])[C:7]3[C:15]([OH:16])=[N:14][N:13]([C:17]4[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=4)[C:12](=[O:25])[C:8]=3[NH:9][C:10]=2[CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3283Diethyl EtherHCID 178492080HCID 178492080, 화합물

생성물 1

HCID 178515074HCID 178515074, 화합물수율 85.9%

시약·촉매·용매 1

HCID 6395Methanesulfonic Acid용매

반응 조건

온도
160 °C

실험 절차

7-Chloro-1-hydroxy-3-(4-methoxyphenyl)-3,4,5,10-tetrahydropyridazino[4,5-b]quinoline-4,10-dione (0.800 g, 2.16 mM) was stirred in methanesulfonic acid (16 mL) to give an amber solution. This solution was heated to 160° C. for 6 hours and cooled to room temperature. Addition of ethyl ether (250 mL) gave a tan precipitate which was stirred for 1 hour. The solid was collected and washed with methanol/ether to give the title compound (0.661 g, 77%) as a tan powder, mp 393-395° C.; MS(CI): 356 (M+H).

후처리

  1. customto give an amber solution
  2. temperaturecooled to room temperature
  3. customgave a tan precipitate which
  4. customThe solid was collected
  5. washwashed with methanol/ether

출처 및 근거

ORD 기록
ord-de1279ac6fae4dc2a05de34d82730489
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06214826B1

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