Hydrochloric Acid → 1-[4-(7-Chloro-4-quinazolinylamino)benzenesulphonyl]-4-methylpiperazine

HRID 570053ノート

反応式

HRID 570053 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(=O)([O-])[O-].[Na+].[Na+].Cl.[Cl:15][C:16]1[CH:25]=[C:24]2[C:19]([C:20]([NH:26][C:27]3[CH:32]=[CH:31][C:30]([S:33](Cl)(=[O:35])=[O:34])=[CH:29][CH:28]=3)=[N:21][CH:22]=[N:23]2)=[CH:18][CH:17]=1.Cl>C(Cl)(Cl)Cl.O.C(O)C>[Cl:15][C:16]1[CH:25]=[C:24]2[C:19]([C:20]([NH:26][C:27]3[CH:28]=[CH:29][C:30]([S:33]([N:5]4[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]4)(=[O:34])=[O:35])=[CH:31][CH:32]=3)=[N:21][CH:22]=[N:23]2)=[CH:18][CH:17]=1

参加物

8

反応物 4

HCID 313Hydrochloric Acid2 回HCID 10340Sodium CarbonateHCID 531671-MethylpiperazineHCID 212739544-(7-Chloro-4-quinazolinylamino)benzenesulphonyl chloride hydrochloride

生成物 1

HCID 135372031-[4-(7-Chloro-4-quinazolinylamino)benzenesulphonyl]-4-methylpiperazine

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒

反応条件

温度
10 °C

実験手順

N-Methylpiperazine (1.0 g, 0.01 mole) was dissolved in chloroform (50 ml). Sodium carbonate (10 g) was dissolved in water (50 ml). The solutions were combined and cooled to 10° C. 4-(7-Chloro-4-quinazolinylamino)benzenesulphonyl chloride hydrochloride (3.85 g, 0.01 mole) was added in portions to the vigorously stirred solution. Stirring was continued for one hour. The chloroform layer was separated, dried and evaporated. The resulting gummy solid was redissolved in chloroform and chromatographed on an alumina column. Elution with chloroform gave a first band which was discarded. The second band was obtained as a low melting solid, which was converted to the hydrochloride by dissolving in ethanol and adding ethereal hydrogen chloride to give the title compound as the sesquihydrochloride (650 mg) m.p. 237°-239° C.

後処理

  1. customThe chloroform layer was separated
  2. customdried
  3. customevaporated
  4. dissolutionThe resulting gummy solid was redissolved in chloroform
  5. customchromatographed on an alumina column
  6. washElution with chloroform
  7. customgave a first band which
  8. customThe second band was obtained as a low melting solid, which

出典と根拠

ORDレコード
ord-067f969d2e5d4976854d945aa56161e4
出典データセット
uspto-grants-1988_03
特許番号
US04734510

反応ノート

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