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Sodium Carbonate → HCID 13236381、化合物

HRID 1649256
ノート
印刷プレビュー

反応式

HRID 1649256 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])[CH2:8][CH2:7]2.Br.[Br:14][CH2:15][CH2:16][NH:17][CH2:18][CH2:19]Br.C(=O)([O-])[O-].[Na+].[Na+]>CO>[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])[CH2:8][CH2:7]3)[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 12692731Ethanamine, 2-bromo-N-(2-bromoethyl)-, hydrobromide (1:1)HCID 133171138-Amino-3,4-dihydro-2(1H)-quinolinone

生成物 1

HCID 13236381HCID 13236381、化合物収率 16.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

8-Amino-3,4-dihydrocarbostyril (7.5 g, 46.2 mmols) and bis(β-bromoethyl)amine hydrobromide (15.9 g, 50.8 mmols) were suspended in methanol and the suspension was heated under reflux while stirring for 9 hours. After adding 2.5 g of sodium carbonate, the reaction mixture was further heated under reflux for 8 hours while stirring, and stirred on an ice bath for 1 hours. Crystals which precipitated were collected by filtration. The crude crystals thus obtained were recrystallized from methanol-ether to give 2.4 g of 8-(1-piperazinyl)-3,4-dihydrocarbostyril hydrobromide, m.p. above 300° C., colorless needles.

後処理

  1. temperaturethe suspension was heated
  2. temperatureunder reflux
  3. temperaturethe reaction mixture was further heated
  4. temperatureunder reflux for 8 hours
  5. stirringwhile stirring
  6. stirringstirred on an ice bath for 1 hours
  7. customCrystals which precipitated
  8. filtrationwere collected by filtration
  9. customThe crude crystals thus obtained
  10. customwere recrystallized from methanol-ether

出典と根拠

ORDレコード
ord-0338ebd2647f42cdbaa7cfeb7c846732
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04415572

反応ノート

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