Diisopropylethylamine → 6-[4-(2-Pyrrolidin-1-ylethyl)piperazin-1-yl]pyrimidin-4-amine

HRID 1241377ノート

反応式

HRID 1241377 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=1.C(N(C(C)C)CC)(C)C.[N:18]1([CH2:23][CH2:24][N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[CH2:22][CH2:21][CH2:20][CH2:19]1>C(O)CCC>[N:18]1([CH2:23][CH2:24][N:25]2[CH2:26][CH2:27][N:28]([C:2]3[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=3)[CH2:29][CH2:30]2)[CH2:19][CH2:20][CH2:21][CH2:22]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2380124-Amino-6-chloropyrimidineHCID 27372501-[2-(Pyrrolidin-1-yl)ethyl]piperazine

生成物 1

HCID 219346496-[4-(2-Pyrrolidin-1-ylethyl)piperazin-1-yl]pyrimidin-4-amine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
125 °C

実験手順

6-Chloropyrimidin-4-amine 7-2 (0.317 g, 2.44 mmol) and diisopropylethylamine (0.0.316 g, 2.44 mmol) were suspended in n-butanol and 1-(2-pyrrolidin-1-ylethyl)piperazine 11-1 (0.448 g, 2.44 mmol) was added. The reaction was stirred at 125° C. for 18 hours. Upon cooling the reaction was purified on a silica column (DCM:MeOH:NH4OH) to afford 11-2. 1NMR (CD3OD): 7.96 ppm (s, 1H); 5.71 ppm (s, 1H); 3.53 ppm (t, 4H); 2.69 ppm (m, 2H); 2.58 ppm (m, 10H); 1.82 ppm (m, 4H).

後処理

  1. temperatureUpon cooling the reaction
  2. customwas purified on a silica column (DCM:MeOH:NH4OH)
  3. customto afford 11-2

出典と根拠

ORDレコード
ord-86e2bc29a3ef429b8a098b699590e615
出典データセット
uspto-grants-2006_10
特許番号
US07115597B2

反応ノート

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