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

反応式

HRID 2255039 の反応式
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]

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 178506447HCID 178506447、化合物触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3c4625f8dac140a8ae6125b70e51b7a5
出典データセット
uspto-grants-1993_08
特許番号
US05238936

関連ノート

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