Nitrogen → 1-Chloro-4-ethyl-6-methoxy-phthalazine

HRID 2297404ノート

反応式

HRID 2297404 の反応式
[CH2:1]([C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6](=O)[NH:5][N:4]=1)[CH3:2].N#N.P(Cl)(Cl)([Cl:20])=O.C([O-])([O-])=O.[Na+].[Na+]>C(#N)C.O>[Cl:20][C:6]1[C:7]2[C:12](=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)[C:3]([CH2:1][CH3:2])=[N:4][N:5]=1

参加物

7

反応物 4

HCID 947NitrogenHCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 183816114-ethyl-6-methoxy-2H-phthalazin-1-one

生成物 1

HCID 183816451-Chloro-4-ethyl-6-methoxy-phthalazine収率 89%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

A suspension of 4-ethyl-6-methoxy-2H-phthalazin-1-one (1.3 g, 6.76 mmoles), prepared as described in example 9, in dry acetonitrile (20 ml), under stirring and dry N2 at room temperature, was added with phosphorous oxychloride (2.07 g, 13.52 mmoles). The mixture was refluxed and after 2 hours cooled, brought to small volume, taken up in water, added with Na2CO3 in excess and extracted three times with CH2Cl2. The organic phases were anhydrified and brought to dryness to give 1.34 g of the title compound (yield: 89%).

後処理

  1. customprepared
  2. temperatureThe mixture was refluxed and after 2 hours
  3. temperaturecooled
  4. extractionextracted three times with CH2Cl2

出典と根拠

ORDレコード
ord-b4c04b0586874ccbaace943eea67512b
出典データセット
uspto-grants-2002_12
特許番号
US06492360B1

反応ノート

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