Cyanide → HCID 53467828、化合物

HRID 2401169ノート

反応式

HRID 2401169 の反応式
Br[C:2]1[C:3]([NH2:18])=[N:4][C:5]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)=[N:6][C:7]=1[N:8]1[CH:12]=[CH:11][CH:10]=[N:9]1.[C-:19]#[N:20].C(OCC)(=O)C>N1C=CC=CC=1>[NH2:18][C:3]1[C:2]([C:19]#[N:20])=[C:7]([N:8]2[CH:12]=[CH:11][CH:10]=[N:9]2)[N:6]=[C:5]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)[N:4]=1

参加物

5

反応物 3

HCID 5975CyanideHCID 8857Ethyl AcetateHCID 534669585-bromo-2,6-di(1H-pyrazol-1-yl)pyrimidin-4-amine

生成物 1

HCID 53467828HCID 53467828、化合物収率 39.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 0.2 g (0.65 mmol) of 5-bromo-2,6-di(1H-pyrazol-1-yl)pyrimidin-4-amine and 0.06 g (0.72 mmol) of cupper (I) cyanide in 3 ml of pyridine was irradiated with microwaves at 250° C. for 20 min. After nearly complete conversion to the corresponding carbonitrile as was indicated by TLC, ethyl acetate was added and filtered throw celite. The solution was extracted two times with 10 ml of saturated solution of NaHCO3 and Brine. The organic layer was separated, dried with MgSO4 and concentrated to give 0.065 g (39.6%) of the desired product.

後処理

  1. customwas irradiated with microwaves at 250° C. for 20 min
  2. additionwas added
  3. filtrationfiltered
  4. extractionThe solution was extracted two times with 10 ml of saturated solution of NaHCO3 and Brine
  5. customThe organic layer was separated
  6. dry with materialdried with MgSO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-8b7352c0616d400a96ca13f3e0890d8c
出典データセット
uspto-grants-2014_08
特許番号
US08796284B2

反応ノート

読み込み中…