Acetyl chloride → HCID 178474362、化合物

HRID 1443103ノート

反応式

HRID 1443103 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[OH:8].C(N(C(C)C)C(C)C)C.[C:18](Cl)(=[O:20])[CH3:19]>ClCCl>[OH:8][C:7]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[NH:1][C:18](=[O:20])[CH3:19]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 2333923-Amino-4-hydroxypyridine

生成物 1

HCID 178474362HCID 178474362、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

3-Amino-pyridin-4-ol (15.0, 136 mmol) was suspended in 200 ml dichloromethane and N-ethyldiisopropylamine (82 ml, 477 mmol) was added. A solution of acetylchloride (10.6 ml, 150 mmol) in 150 ml dichloromethane was added dropwise at ambient temperature. The reaction mixture was stirred at reflux for 3 hrs and evaporated to dryness. The residue was stirred in methanol and filtered. The solvent was evaporated and the desired product was obtained as a white solid (7.2 g, 35%), MS: m/e=151.1 (M+H+).

後処理

  1. temperatureat reflux for 3 hrs
  2. customevaporated to dryness
  3. stirringThe residue was stirred in methanol
  4. filtrationfiltered
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-ef7202db79e244bfb772d3d212c18bbe
出典データセット
uspto-grants-2010_02
特許番号
US07659401B2

反応ノート

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