3-(Trifluoromethyl)benzaldehyde → HCID 89445371, 화합물

HRID 632728노트

반응식

HRID 632728 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([NH2:20])=[N:10][CH:11]=[N:12][C:13]=2[N:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)=[CH:4][CH:3]=1.[F:21][C:22]([F:32])([F:31])[C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH:26]=O.C[Si]([C:37]#[N:38])(C)C>C(#N)C>[NH2:20][C:9]1[N:10]=[CH:11][N:12]=[C:13]([N:14]2[CH2:19][CH2:18][N:17]([CH:26]([C:25]3[CH:28]=[CH:29][CH:30]=[C:23]([C:22]([F:32])([F:31])[F:21])[CH:24]=3)[C:37]#[N:38])[CH2:16][CH2:15]2)[C:8]=1[C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1

참가 물질

5

반응물 3

HCID 679903-(Trifluoromethyl)benzaldehydeHCID 82115Trimethylsilyl cyanideHCID 89442443HCID 89442443, 화합물

생성물 1

HCID 89445371HCID 89445371, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In a round bottom flask equipped with a stir bar was dissolved 5-(4-Fluoro-phenyl)-6-piperazin-1-yl-pyrimidin-4-ylamine (1 eq) and 3-trifluoromethyl-benzaldehyde (1.05 eq) in acetonitrile. The vial was sealed with a rubber septa, then evacuated and backfilled with argon. To this sealed vessel was added trimethylsilyl cyanide (1.05 eq) and the reaction was allowed to stir at room temperature until complete. The reaction is quenched by addition of an equal amount of ammonium chloride (saturated, aqueous solution), then extracted with ethyl acetate. The organic layers are then dried over sodium sulfate, filtered and concentrated to give the title compound. LC-MS: (M+1=457, obsd.=457).

후처리

  1. customIn a round bottom flask equipped with a stir bar
  2. customThe vial was sealed with a rubber septa
  3. customevacuated
  4. customThe reaction is quenched by addition of an equal amount of ammonium chloride (saturated, aqueous solution)
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layers are then dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-39c2c078c0af47019cf0441dbfaf624f
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321760B2

반응 노트

불러오는 중…