Dimethylformamide → 4-Chloro-7-methoxycinnoline hydrochloride

HRID 7485ノート

反応式

HRID 7485 の反応式
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

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 178418974HCID 178418974、化合物

生成物 1

HCID 219910204-Chloro-7-methoxycinnoline hydrochloride収率 97%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6d4c3752ba7f4c5eae803cc519e25ef9
出典データセット
uspto-grants-2006_08
特許番号
US07087602B2

反応ノート

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