Piperazine → 1-(10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazine

HRID 36611

反応式

HRID 36611 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][CH2:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2>C1COCC1.C(Cl)Cl>[N:1]1([CH:8]2[C:9]3[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=3[CH2:11][CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]2=3)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 4837PiperazineHCID 145875H-Dibenzo(a,d)cycloheptene, 10,11-dihydro-5-chloro-

生成物 1

HCID 27359361-(10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazine収率 2,915.9%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Into a solution of partially dissolved piperazine (15.2 g, 0.17 mmol) in THF (130 mL) at more temperature was added dropwise a solution of 5-chloro-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2.3g, 10.3 mmol) in 20 mL THF. The reaction was allowed to stir overnight and then was diluted with CH2Cl2, washed once with 1.0N NaOH solution, once with brine and then dried (Mg SO4). It was then filtered and the solvent removed to give a residue which was flash chromatographed (5% MeOH saturated with NH3 in CH2Cl2) to give 1.38 g of a glassy solid of the title compound.

後処理

  1. washwashed once with 1.0N NaOH solution, once with brine
  2. dry with materialdried (Mg SO4)
  3. filtrationIt was then filtered
  4. customthe solvent removed
  5. customto give a residue which
  6. customchromatographed (5% MeOH saturated with NH3 in CH2Cl2)

出典と根拠

ORDレコード
ord-70f3f48392af48ca9feb3ad8a30df0a3
出典データセット
uspto-grants-1995_05
特許番号
US05416087

関連ノート

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