Triethylamine → HCID 131716831、化合物

HRID 1030614ノート

反応式

HRID 1030614 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][NH2:16])[CH2:9][CH2:8]1.[C:17]12([C:27]([Cl:29])=[O:28])[CH2:26][CH:21]3[CH2:22][CH:23]([CH2:25][CH:19]([CH2:20]3)[CH2:18]1)[CH2:24]2.C(N(CC)CC)C>C(Cl)Cl>[OH2:28].[ClH:29].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][NH:16][C:27]([C:17]23[CH2:26][CH:21]4[CH2:20][CH:19]([CH2:25][CH:23]([CH2:22]4)[CH2:24]2)[CH2:18]3)=[O:28])[CH2:9][CH2:8]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 989151-Adamantanecarbonyl chlorideHCID 107042273-(4-Pyrimidin-2-ylpiperazin-1-yl)propan-1-amine

生成物 1

HCID 131716831HCID 131716831、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of [4-(2-pyrimidinyl)piperazinyl]propylamine (1.12 g, 0.005 mol) in 50 mL of methylene chloride, adamantane-1-carboxylic acid chloride (1 g, 0.005 mol) and triethylamine (1.0 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 a column of silica gel and ethyl acetate as the eluent. The title compound was separated and converted to the hydrochloride, hydrate salt with ethanolic HCl (1.6 g), m.p. 146°-148° 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-340223c5e9f64d51a56a1cc4055b6b9b
出典データセット
uspto-grants-1992_04
特許番号
US05106849

反応ノート

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