Sodium Carbonate → HCID 13236375、化合物

HRID 1649257ノート

反応式

HRID 1649257 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH:8]=[CH:7]2.Br.[Br:14][CH2:15][CH2:16][NH:17][CH2:18][CH2:19]Br.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C>[BrH:14].[N:1]1([C:2]2[CH:3]=[CH:4][CH:5]=[C:6]3[C:11]=2[NH:10][C:9](=[O:12])[CH:8]=[CH:7]3)[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 12692731Ethanamine, 2-bromo-N-(2-bromoethyl)-, hydrobromide (1:1)HCID 133171128-Aminoquinolin-2(1H)-one

生成物 1

HCID 13236375HCID 13236375、化合物収率 17%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

8-Aminocarbostyril (15.47 g, 96.6 mmols) and bis(β-bromoethyl)amine hydrobromide (33 g, 106 mmols) were suspended in DMF and the suspension was stirred at 70° to 80° C. for 10 hours. After adding 5.1 g of sodium carbonate the reaction mixture was stirred at the same temperature as above for 7 hours. After distilling off the solvent under reduced pressure, methanol was added to the residue to crystallize. The crude crystals thus obtained were recrystallized from methanol-ether to give 5.1 g of 8-(1-piperazinyl)carbostyril hydrobromide, m.p. above 300° C., colorless scales.

後処理

  1. stirringwas stirred at the same temperature as above for 7 hours
  2. distillationAfter distilling off the solvent under reduced pressure, methanol
  3. additionwas added to the residue
  4. customto crystallize
  5. customThe crude crystals thus obtained
  6. customwere recrystallized from methanol-ether

出典と根拠

ORDレコード
ord-f59ee3fb5da545a8bae2259602b057d7
出典データセット
uspto-grants-1983_11
特許番号
US04415572

反応ノート

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