Cyanide → HCID 53467828, 화합물

HRID 2401169노트

반응식

HRID 2401169 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 53467828HCID 53467828, 화합물수율 39.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8b7352c0616d400a96ca13f3e0890d8c
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796284B2

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