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

HRID 2268833노트

반응식

HRID 2268833 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 183816451-Chloro-4-ethyl-6-methoxy-phthalazine수율 89%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-687c15e315844155ac11d7ef40e0aae8
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329370B1

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