Hydrazine hydrate (1:1) → 4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one

HRID 2268855노트

반응식

HRID 2268855 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH:8]=[C:9]1[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[C:11](=O)[O:10]1.O.[NH2:23][NH2:24]>CO>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[C:11](=[O:10])[NH:24][N:23]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 54395392HCID 54395392, 화합물

생성물 1

HCID 224827114-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one수율 80%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 3-(3,5-dichloro-pyridin-4-ylmethylene)-6-methoxy-3H-isobenzofuran-1-one (84.4 g, 0.126 mole), prepared as described in example 37, in CH3OH (200 ml) under N2 was added with hydrazine monohydrate (18.4 ml, 0.378 mole). The mixture was refluxed for 1 hour, then left overnight at room temperature and cooled over ice. The solid was filtered, washed with cold CH3OH and dried in oven at 50° C. under vacuum; 33.3 g of the title compound were thus obtained (yield: 80%). m.p.: 259-262° C.

후처리

  1. customprepared
  2. temperatureThe mixture was refluxed for 1 hour
  3. temperaturecooled over ice
  4. filtrationThe solid was filtered
  5. washwashed with cold CH3OH
  6. customdried in oven at 50° C. under vacuum

출처 및 근거

ORD 기록
ord-de5bc3bb59bf45efa7f95d7cfc09dd6f
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329370B1

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