Sodium Carbonate → 1-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine

HRID 1699445

反応式

HRID 1699445 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][CH2:7]2.Cl.Cl[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[CH2:7]1[C:8]2[C:3](=[C:2]([N:1]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[CH:11]=[CH:10][CH:9]=2)[CH2:4][CH2:5][CH2:6]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 166715-TetralinylamineHCID 522769Bis(2-chloroethyl)amine hydrochloride

生成物 1

HCID 986981-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine収率 50%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

14.7 g (0.1 mol) of 5-aminotetralin were refluxed with 18 g (0.11 mol) of bis(β-chloroethyl)amine hydrochloride in 300 ml of n-butanol for 48 h and, after cooling, 5.4 g of sodium carbonate were added and the mixture was refluxed for a further 20 h. The precipitate which formed on cooling was filtered off with suction and taken up in water, and 2N sodium hydroxide solution was added. The aqueous phase was extracted with ethyl acetate, and washing with water and drying over sodium sulfate were followed by evaporation under reduced pressure. It was possible in this way to isolate 10.7 g (50%) of the product as an oil.

後処理

  1. temperatureafter cooling
  2. temperaturethe mixture was refluxed for a further 20 h
  3. customThe precipitate which formed
  4. temperatureon cooling
  5. filtrationwas filtered off with suction
  6. addition2N sodium hydroxide solution was added
  7. extractionThe aqueous phase was extracted with ethyl acetate
  8. washwashing with water
  9. dry with materialdrying over sodium sulfate
  10. customwere followed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-083b0cff1ad9423e8fbf0b11b60a74c7
出典データセット
uspto-grants-2002_02
特許番号
US06346622B1

関連ノート

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