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

HRID 2394270

반응식

HRID 2394270 반응식
[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.ClCl>[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9]([Cl:15])=[O:11])=[CH:4][N:3]=1

참가 물질

5

반응물 2

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

생성물 1

HCID 212206502-Chloro-4-methylpyrimidine-5-carbonyl chloride수율 61.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 24526Chlorine용매

실험 절차

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 CH2 Cl2 (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; 1HNMR (CDCl3) δ d 9.02 (s, 1H), 2.74 (s, 3H).

후처리

  1. concentrationThe solution was concentrated
  2. distillationdistilled

출처 및 근거

ORD 기록
ord-b5caa985263a478b8528cb22f5b22d33
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05811428

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