3-(Trifluoromethyl)benzaldehyde → HCID 89445371、化合物

HRID 632728ノート

反応式

HRID 632728 の反応式
[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

参加物

5

反応物 3

HCID 679903-(Trifluoromethyl)benzaldehydeHCID 82115Trimethylsilyl cyanideHCID 89442443HCID 89442443、化合物

生成物 1

HCID 89445371HCID 89445371、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-39c2c078c0af47019cf0441dbfaf624f
出典データセット
uspto-grants-2016_04
特許番号
US09321760B2

反応ノート

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