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

HRID 1060585노트

반응식

HRID 1060585 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-a80c100b29034a9caab5a688b6c27a70
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525055B1

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