Oxalyl chloride → 6-Chloro-4-pyrimidinecarboxylic acid

HRID 880329

반응식

HRID 880329 반응식
O[C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8]([OH:10])=[O:9])[CH:3]=1.C(Cl)(C([Cl:15])=O)=O>CCOC(C)=O.CN(C=O)C>[Cl:15][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8]([OH:10])=[O:9])[CH:3]=1

참가 물질

5

반응물 2

HCID 65578Oxalyl chlorideHCID 178524636HCID 178524636, 화합물

생성물 1

HCID 166377476-Chloro-4-pyrimidinecarboxylic acid수율 92.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 8857Ethyl Acetate용매

반응 조건

온도
75 °C

실험 절차

To a solution of 6-hydroxypyrimidine-4-carboxylic acid (6.0 g, 42.8 mmol) in EtOAc (90 mL) was added (COCl)2 (12 mL) dropwise, followed by a few drops of DMF. The mixture was stirred at 75° C. for 3 h, and then at 25° C. for 16 h. The solvent was evaporated to give the crude 6-chloropyrimidine-4-carboxylic acid (6.3 g, yield: 92.9%). 1H NMR (400 MHz, DMSO-d6) δ 8.31 (s, 1H), 6.88 (s, 1H).

후처리

  1. waitat 25° C. for 16 h
  2. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-92a225dc2b3c44f69e074e123efa6597
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993555B2

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