Sulfanilamide → 4-[(8-Bromo-6-fluoro-2-quinazolinyl)amino]benzenesulfonamide

HRID 2079636ノート

反応式

HRID 2079636 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:13])[CH:5]=[C:6]2[C:11]=1[N:10]=[C:9](Cl)[N:8]=[CH:7]2.[NH2:14][C:15]1[CH:20]=[CH:19][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[CH:17][CH:16]=1.C(OCC)(=O)C>C(O)(C)C>[Br:1][C:2]1[CH:3]=[C:4]([F:13])[CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([S:21]([NH2:24])(=[O:22])=[O:23])=[CH:17][CH:16]=1)[N:8]=[CH:7]2

参加物

5

反応物 3

HCID 5333SulfanilamideHCID 8857Ethyl AcetateHCID 591992998-Bromo-2-chloro-6-fluoroquinazoline

生成物 1

HCID 250162634-[(8-Bromo-6-fluoro-2-quinazolinyl)amino]benzenesulfonamide収率 81%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
120 °C

実験手順

To a 0.4M suspension of 8-bromo-2-chloro-6-fluoroquinazoline in isopropanol was added 4-aminobenzensulfonamide (1 eq). The reaction mixture was heated to 120° C. in an oil bath for 2 days. LCMS showed that reaction was complete under the condition. Ethyl acetate was added to the reaction flask and the suspension was stirred at ambient temperature for 30 min and was filtered. Filter cake was rinsed with hexane and dried in vacuum to give product in 81% yield. ES/MS m/z 397/399 (MH+).

後処理

  1. customLCMS showed that reaction
  2. filtrationwas filtered
  3. filtrationFilter cake
  4. washwas rinsed with hexane
  5. customdried in vacuum
  6. customto give product in 81% yield

出典と根拠

ORDレコード
ord-23d7a533e393465fa320ea2cc31c2812
出典データセット
uspto-grants-2011_04
特許番号
US07932262B2

反応ノート

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