Sodium Carbonate → HCID 13236375, 화합물

HRID 1649257노트

반응식

HRID 1649257 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 13236375HCID 13236375, 화합물수율 17%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f59ee3fb5da545a8bae2259602b057d7
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04415572

반응 노트

불러오는 중…