Hydrazine hydrate (1:1) → [4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-phthalazin-1-yl]-hydrazine

HRID 1060585ノート

反応式

HRID 1060585 の反応式
O.[NH2:2][NH2:3].Cl[C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH3:16])[CH:13]=2)[C:8]([CH2:17][C:18]2[C:23]([Cl:24])=[CH:22][N:21]=[CH:20][C:19]=2[Cl:25])=[N:7][N:6]=1>C(O)C>[Cl:25][C:19]1[CH:20]=[N:21][CH:22]=[C:23]([Cl:24])[C:18]=1[CH2:17][C:8]1[C:9]2[C:14](=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[C:5]([NH:2][NH2:3])=[N:6][N:7]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 186292104-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine

生成物 1

HCID 18629212[4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-phthalazin-1-yl]-hydrazine収率 109.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Hydrazine hydrate (0.81 ml, 0.84 g, 16.8 mmoles) was added to a solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (2 g, 5.6 mmoles), obtained as described in example 13, in ethanol (30 ml), and the mixture was kept under reflux for 24 hours, then cooled in ice and the resultant precipitate was filtered, washed with ethanol and ethyl ether and dried under vacuum at 50° C. to give 2.14 g of the title compound (stoichiometric yield). m.p.: 297-299° C.

後処理

  1. customobtained
  2. temperatureunder reflux for 24 hours
  3. temperaturecooled in ice
  4. filtrationthe resultant precipitate was filtered
  5. washwashed with ethanol and ethyl ether
  6. customdried under vacuum at 50° C.

出典と根拠

ORDレコード
ord-a80c100b29034a9caab5a688b6c27a70
出典データセット
uspto-grants-2003_02
特許番号
US06525055B1

反応ノート

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