Trifluoroacetic acid → (6-Bromo-pyridazin-3-yl)-(4-chloro-benzyl)-amine

HRID 1024230

反応式

HRID 1024230 の反応式
[Br:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:17]=[CH:16][C:13]([CH:14]=O)=[CH:12][CH:11]=1.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>C(#N)C.O>[Br:1][C:2]1[N:7]=[N:6][C:5]([NH:8][CH2:14][C:13]2[CH:16]=[CH:17][C:10]([Cl:9])=[CH:11][CH:12]=2)=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 6422Trifluoroacetic acidHCID 77264-ChlorobenzaldehydeHCID 12052TriethylsilaneHCID 27947796-Bromopyridazin-3-amine

生成物 1

HCID 57619288(6-Bromo-pyridazin-3-yl)-(4-chloro-benzyl)-amine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To 6-bromo-pyridazin-3-ylamine (521, 0.85 g, 0.0049 mol) in acetonitrile (30.0 mL) were added 4-chlorobenzaldehyde (40, 0.82 g, 0.0058 mol), triethylsilane (4.0 mL, 0.025 mol) and trifluoroacetic acid (2.0 mL, 0.026 mol). The reaction was heated to reflux for 4 hours, then poured into water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated and washed with ethyl acetate to give a white solid (522, 1.0 g). MS (ESI) [M+H+]+=298.3, 300.2.

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 4 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. washwashed with ethyl acetate
  9. customto give a white solid (522, 1.0 g)

出典と根拠

ORDレコード
ord-ccf63b55d30f4df48f622b0cd923c1d1
出典データセット
uspto-grants-2014_05
特許番号
US08722702B2

関連ノート

読み込み中…