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Methanesulfonic Acid → HCID 178492080、化合物

HRID 1977199
ノート
印刷プレビュー

反応式

HRID 1977199 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178492080HCID 178492080、化合物収率 44%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 C18H12ClN3O4: Calculated: C, 58.50; H, 3.27; N, 11.36; Found: C, 58.30; H, 3.41; N, 10.92;

後処理

  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

出典と根拠

ORDレコード
ord-d5dcdd74dede4e609426bc4593525efd
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06232313B1

反応ノート

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