Triethylamine → HCID 19826117、化合物

HRID 583358ノート

反応式

HRID 583358 の反応式
[CH2:1]([NH:3][CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)[CH3:2].C(N(CC)CC)C.[C:18](Cl)(=[O:21])[CH:19]=[CH2:20]>>[CH2:1]([N:3]([CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)[C:18](=[O:21])[CH:19]=[CH2:20])[CH3:2]

参加物

4

反応物 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 96681N-Ethylpyridine-4-methylamine

生成物 1

HCID 19826117HCID 19826117、化合物収率 68.4%

実験手順

To a 0° C. solution of 0.835 ml (6.0 mmol) of 4-(ethylaminomethyl) pyridine and 1.05 ml (7.5 mmol) of triethylamine in 10 ml dichloomethane, was dropwise added 0.406 ml (5.0 mmol) of acryloyl chloride. The reaction mixture was warmed to room temperature and stilred for 18 hr. The resulting nmxture was washed with water and brne, dried over MgSO4, filtered and concentrated in vacuo. The residue was chromatographed on silica gel with 3% MeOH/CH2Cl2 as the eluant to provide 651 mg (68%) of the desired product as a yellow gum. Electrospray Mass Spec 191(M+H).

後処理

  1. customTo a 0° C.
  2. washThe resulting nmxture was washed with water and brne
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on silica gel with 3% MeOH/CH2Cl2 as the eluant

出典と根拠

ORDレコード
ord-b9aa764d069a4be2aed42a96c1eef3ab
出典データセット
uspto-grants-1999_07
特許番号
US05929097

反応ノート

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