Diisopropylethylamine → (S)-4-{6-Chloro-2-[1-(4-fluorophenyl)ethylamino]pyrimidin-4-yl}piperazine-2,6-dione

HRID 1187684ノート

反応式

HRID 1187684 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=1.[NH:19]1[C:24](=[O:25])[CH2:23][NH:22][CH2:21][C:20]1=[O:26].C(N(CC)C(C)C)(C)C>O1CCCC1.CN(C)C=O.C(OCC)(=O)C>[Cl:8][C:6]1[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=[C:2]([N:22]2[CH2:23][C:24](=[O:25])[NH:19][C:20](=[O:26])[CH2:21]2)[CH:7]=1

参加物

7

反応物 3

HCID 81531DiisopropylethylamineHCID 338690Piperazine-2,6-dioneHCID 86659372HCID 86659372、化合物

生成物 1

HCID 86659384(S)-4-{6-Chloro-2-[1-(4-fluorophenyl)ethylamino]pyrimidin-4-yl}piperazine-2,6-dione収率 58.8%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

182 mg of (S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine (Reference Example 1) and 80 mg of piperazine-2,6-dione were dissolved in 2 ml of tetrahydrofuran and 2 ml of N,N-dimethylformamide, and 122 μl of N,N-diisopropylethylamine was added thereto, and the mixture was stirred at 80° C. for 32 hours. The reaction solution was air-cooled to room temperature, and then diluted with ethyl acetate. The solution was washed with water and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 136 mg of the objective compound as white powder.

後処理

  1. temperatureThe reaction solution was air-cooled to room temperature
  2. washThe solution was washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a79bdee204fa4a10b4da810c19c19701
出典データセット
uspto-grants-2014_03
特許番号
US08673891B2

反応ノート

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