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

HRID 36611

반응식

HRID 36611 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-70f3f48392af48ca9feb3ad8a30df0a3
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416087

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