Hydrazine hydrate (1:1) → 3-chloro-4-cyclobutyl-6-hydrazinylPyridazine

HRID 380322

반응식

HRID 380322 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1.O.[NH2:14][NH2:15]>O1CCOCC1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:14][NH2:15])=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 219732193,6-Dichloro-4-cyclobutylpyridazine

생성물 1

HCID 226099463-chloro-4-cyclobutyl-6-hydrazinylPyridazine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

3,6-Dichloro-4-cyclobutylpyridazine (22.5 g, 0.11 mol) and hydrazine hydrate (34 ml, 0.66 mol) were heated at reflux in dioxane (280 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (13.3 g, 64%). 1H NMR (250 MHz , d6-DMSO) 1.68-1.86 (1H, m), 2.00-2.11 (3H, m), 2.29-2.38 (2H, m), 3.52-3.61 (1H, m), 4.35 (2H, br), 6.99 (1H, s), 8.06 (1H, br); MS (ES+) m/e 198 [MH]+, 200 [MH]+.

후처리

  1. temperatureUpon cooling the desired isomer
  2. customcrystallized from the reaction
  3. filtrationwas collected by filtration (13.3 g, 64%)

출처 및 근거

ORD 기록
ord-ee749b0974f94195a9d027d4446f3588
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303605B1

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