(S)-2-Benzylpiperazine → HCID 20816900、化合物

HRID 897416ノート

反応式

HRID 897416 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:12]2[N:13]([CH:25]=[N:26][N:27]=2)[C:14](SC)=[N:15][C:16]=1[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1.[CH2:28]([C@H:35]1[CH2:40][NH:39][CH2:38][CH2:37][NH:36]1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>CN(C=O)C>[CH2:28]([C@@H:35]1[NH:36][CH2:37][CH2:38][N:39]([C:14]2[N:13]3[CH:25]=[N:26][N:27]=[C:12]3[C:11]([C:2]3[CH:3]=[CH:4][C:5]4[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=4)[CH:1]=3)=[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)[N:15]=2)[CH2:40]1)[C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

参加物

4

反応物 2

HCID 20760001(S)-2-BenzylpiperazineHCID 22346600HCID 22346600、化合物

生成物 1

HCID 20816900HCID 20816900、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

8-(2-naphthyl)-5-methylthio-7-(4-pyridyl)-1,2,4-triazolo[4,3-c]pyrimidine (200 mg, 0.54 mmol), K3CO3 (100 mg) and (S)-2-benzylpiperazine (170 mg, 0.97 mmol) were combined in dry DMF (ca. 4 mL) and the mixture was heated at 100° C. for 48 h. The reaction was cooled to RT, and partitioned between water and ethyl acetate. The organic layer was dried over Na2SO4 and then concentrated in vacuo. The residue was purified by flash chromatography (2-8% MeOH/NH3:CH2Cl2) to provide the product as a tan solid; MS (m/z) 498.3 (M+H)+; C31H27N7 requir. 497.59.

後処理

  1. temperatureThe reaction was cooled to RT
  2. custompartitioned between water and ethyl acetate
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography (2-8% MeOH/NH3:CH2Cl2)

出典と根拠

ORDレコード
ord-6c46afab90814b499da3d651e4445c6c
出典データセット
uspto-grants-2005_07
特許番号
US06921762B2

反応ノート

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