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

HRID 2268855ノート

反応式

HRID 2268855 の反応式
[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

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 54395392HCID 54395392、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de5bc3bb59bf45efa7f95d7cfc09dd6f
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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