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Triethylamine → N-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyl]tricyclo[3,3,1,13,7]decane-1-carboxamide Dihydrochloride Sesquihydrate

HRID 1197834
ノート
印刷プレビュー

反応式

HRID 1197834 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][NH2:17])[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[C:18]12([C:28]([Cl:30])=[O:29])[CH2:27][CH:22]3[CH2:23][CH:24]([CH2:26][CH:20]([CH2:21]3)[CH2:19]1)[CH2:25]2.C(N(CC)CC)C>C(Cl)Cl>[OH2:29].[ClH:1].[ClH:30].[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17][C:28]([C:18]34[CH2:27][CH:22]5[CH2:21][CH:20]([CH2:26][CH:24]([CH2:23]5)[CH2:25]3)[CH2:19]4)=[O:29])[CH2:12][CH2:13]2)[CH:5]=[CH:6][CH:7]=1.[OH2:29].[OH2:29].[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17][C:28]([C:18]34[CH2:27][CH:22]5[CH2:21][CH:20]([CH2:26][CH:24]([CH2:23]5)[CH2:25]3)[CH2:19]4)=[O:29])[CH2:12][CH2:13]2)[CH:5]=[CH:6][CH:7]=1.[ClH:1].[ClH:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 989151-Adamantanecarbonyl chlorideHCID 35067593-[4-(3-Chlorophenyl)piperazin-1-yl]propan-1-amine

生成物 1

HCID 131717306N-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyl]tricyclo[3,3,1,13,7]decane-1-carboxamide Dihydrochloride Sesquihydrate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of [4-(3-chlorophenyl)piperazinyl]propylamine (1.28 g, 0.005 mol) in 50 mL of methylene chloride, adamantane-1-carboxylic acid chloride (1 g, 0.005 mol) and triethylamine (1 g, 0.01 mol) were added. Stirring was continued at room temperature overnight. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The remaining residue was subjected to preparative HPLC using silica gel column and ethyl acetate as the eluent. The title compound was separated and converted to the dihydrochloride salt with ethanolic HCl (1.5 g), m.p. 209°-210° C.

後処理

  1. washThe methylene chloride solution was washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. customevaporated under reduced pressure
  4. customThe title compound was separated

出典と根拠

ORDレコード
ord-e08f77cb09c84f7ba360787b619964ff
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05278160

反応ノート

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