Ammonia → 2,4-Diallylamino-6-{2-[4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazin-1-yl]ethylamino}-1,3,5-triazine

HRID 2255039

반응식

HRID 2255039 반응식
C(O)(=O)/C=C/C(O)=O.C(O)(=O)/C=C/C(O)=O.[CH2:17]([NH:20][C:21]1[N:26]=[C:25]([NH:27][CH2:28][CH:29]=[CH2:30])[N:24]=[C:23]([NH:31][CH2:32][CH2:33][N:34]2[CH2:39][CH2:38][N:37]([CH:40]3[C:46]4[CH:47]=[CH:48][CH:49]=[CH:50][C:45]=4[CH2:44][CH2:43][C:42]4[CH:51]=[CH:52][CH:53]=[CH:54][C:41]3=4)[CH2:36][CH2:35]2)[N:22]=1)[CH:18]=[CH2:19].N>C(O)C.[H][H].[Ni]>[CH2:28]([NH:27][C:25]1[N:26]=[C:21]([NH:20][CH2:17][CH:18]=[CH2:19])[N:22]=[C:23]([NH:31][CH2:32][CH2:33][N:34]2[CH2:35][CH2:36][N:37]([CH:40]3[C:41]4[CH:54]=[CH:53][CH:52]=[CH:51][C:42]=4[CH2:43][CH2:44][C:45]4[CH:50]=[CH:49][CH:48]=[CH:47][C:46]3=4)[CH2:38][CH2:39]2)[N:24]=1)[CH:29]=[CH2:30]

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 678577352,4-diallylamino-6-{2-[4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazin-1-yl]ethylamino}-1,3,5-triazine difumarate

생성물 1

HCID 149509122,4-Diallylamino-6-{2-[4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazin-1-yl]ethylamino}-1,3,5-triazine

시약·촉매·용매 2

HCID 178506447HCID 178506447, 화합물촉매HCID 702Ethanol용매

실험 절차

When the reaction is complete, the salt is filtered off, the solvent is evaporated and the residue is taken up in ether, washed with water and dried over MgSO4. After evaporation of the ether, the oily residue is chromatographed on 120 g of silica, using the system CH2Cl2 /CH3OH (92/8) as eluant. After evaporation of the eluate, the recovered base is converted into the difumarate in ethanol to yield, ultimately, 7.7 g of 2,4-diallylamino-6-{2-[4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazin-1-yl]ethylamino}-1,3,5-triazine difumarate crystals melting (cap) at 123°-128° C. The aminoethylpiperazine starting material was prepared by reducing the corresponding cyanomethyl compound, [m.p. (cap): 112°-113° C.] with H2 /Ni, in ethanol, in the presence of NH3.

후처리

  1. filtrationthe salt is filtered off
  2. customthe solvent is evaporated
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. customAfter evaporation of the ether
  6. customthe oily residue is chromatographed on 120 g of silica
  7. customAfter evaporation of the eluate
  8. customto yield
  9. custom(cap) at 123°-128° C

출처 및 근거

ORD 기록
ord-3c4625f8dac140a8ae6125b70e51b7a5
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05238936

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