Water → HCID 86633450、化合物

HRID 1668657ノート

反応式

HRID 1668657 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:3]=1.[NH:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]([CH2:24][CH2:25][NH2:26])=[CH:16]1.CCN(C(C)C)C(C)C.O>CC(O)C>[Cl:8][C:6]1[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:3]=[C:2]([NH:26][CH2:25][CH2:24][C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[NH:15][CH:16]=2)[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 1150TryptamineHCID 81531DiisopropylethylamineHCID 120574654,6-dichloro-2-(2-pyridinyl)pyrimidine2 回

生成物 1

HCID 86633450HCID 86633450、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

4,6-Dichloro-2-pyridin-2-yl-pyrimidine (Intermediate F) (1 eq, 8.85 mmol, 2.0 g) and 2-(1H-indol-3-yl)-ethylamine (1 eq, 8.85 mmol, 1.42 g) are dissolved in iPrOH (10 ml). DIPEA (2 eq, 17.7 mmol, 2.29 g) is added and the resulting mixture is heated using microwave radiation at 130° C. for 20 min. The reaction mixture is added to water and extracted with EtOAc. The combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated in vacuo. The crude residue is crystallised from EtOAc giving the title compound [M+H]+=350.

後処理

  1. temperaturethe resulting mixture is heated
  2. customat 130° C.
  3. customfor 20 min
  4. extractionextracted with EtOAc
  5. washThe combined organic layers are washed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue is crystallised from EtOAc giving the title compound [M+H]+=350

出典と根拠

ORDレコード
ord-31020f863ec64a8aa41a32598dba3fda
出典データセット
uspto-grants-2011_08
特許番号
US07989458B2

反応ノート

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