Oxalyl chloride → 2-Chloro-4-methylpyrimidine-5-carbonyl chloride

HRID 1584840

反応式

HRID 1584840 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9]([OH:11])=O)=[CH:4][N:3]=1.C(Cl)(=O)C([Cl:15])=O>CN(C=O)C.C(Cl)Cl>[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9]([Cl:15])=[O:11])=[CH:4][N:3]=1

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 104874142-Chloro-4-methylpyrimidine-5-carboxylic acid

生成物 1

HCID 212206502-Chloro-4-methylpyrimidine-5-carbonyl chloride収率 61.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 2-chloro-4-methylpyrimidine-5-carboxylic acid (0.81 g, 4.70 mmol), oxalyl chloride (0.89 g, 7.05 mmol), DMF (2 drops) in CH2Cl2 (23 mL) was stirred at room temperature under N2 for 4 h. The solution was concentrated and distilled to give the title compound (0.55 g, 61%); b.p. 90-100° C., 1.3 mm/Hg; 1H NMR (CDCl3) δ d9.02 (s, 1H), 2.74 (s, 3H).

後処理

  1. concentrationThe solution was concentrated
  2. distillationdistilled

出典と根拠

ORDレコード
ord-d375475290144e0fa6610171f81d8166
出典データセット
uspto-grants-1999_08
特許番号
US05935966

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