Nitrogen → 1-Chloro-6-methoxyphthalazine

HRID 2268828ノート

反応式

HRID 2268828 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][N:7]=[CH:6]2.N#N.P(Cl)(Cl)([Cl:18])=O>C(#N)C>[Cl:18][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[N:7][N:8]=1

参加物

5

反応物 3

HCID 947NitrogenHCID 24813Phosphorus oxychlorideHCID 122985436-Methoxyphthalazin-1-ol

生成物 1

HCID 183816081-Chloro-6-methoxyphthalazine収率 98.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A suspension of 6-methoxy-2H-phthalazin-1-one (6.4 g, 36.3 mmoles), prepared as described in example 3, in acetonitrile (65 ml) under stirring and dry N2 at room temperature, was dropwise added with phosphorous oxychloride (6.8 ml, 73 mmoles), then the mixture was refluxed. After 3 hours the mixture was concentrated, taken up in water, neutralised with NaHCO3 and extracted more times with CH2Cl2. The organic phases were washed with water, anhydrified and concentrated to give 6.94 g of the title compound (yield: 98.3%). m.p.: 181-183° C.

後処理

  1. customprepared
  2. temperaturethe mixture was refluxed
  3. concentrationAfter 3 hours the mixture was concentrated
  4. extractionextracted more times with CH2Cl2
  5. washThe organic phases were washed with water, anhydrified
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-29f621a189f4445b9ecb0371d7a99b92
出典データセット
uspto-grants-2001_12
特許番号
US06329370B1

反応ノート

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