Dimethylformamide → 4-Chloro-7-methoxycinnoline hydrochloride

HRID 1057339

반응식

HRID 1057339 반응식
O[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[N:4][CH:3]=1.CN(C=O)C.S(Cl)([Cl:21])=O>>[ClH:21].[Cl:21][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[N:4][CH:3]=1

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 178418974HCID 178418974, 화합물

생성물 1

HCID 219910204-Chloro-7-methoxycinnoline hydrochloride수율 97%

실험 절차

The starting material 4-chloro-7-methoxycinnoline hydrochloride was obtained by heating a solution of 4-hydroxy-7-methoxycinnoline (352 mg, 2 mmol), (prepared as described in J. Chem. Soc. 1955, 2100), in thionyl chloride (3.5 ml) containing DMF (20 μl) at reflux, for 1 hour. After removing excess thionyl, chloride by evaporation and azeotroping with toluene. The residue was triturated with ether, filtered off and washed with ether to give 4-chloro-7-methoxycinnoline hydrochloride as a yellow solid (450 mg, 97%).

후처리

  1. temperatureat reflux, for 1 hour
  2. customAfter removing excess thionyl, chloride
  3. customby evaporation
  4. customazeotroping with toluene
  5. customThe residue was triturated with ether
  6. filtrationfiltered off
  7. washwashed with ether

출처 및 근거

ORD 기록
ord-56cabee775524ef88048e4fa63f70c35
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06514971B1

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