Hydrazine hydrate (1:1) → HCID 178432134, 화합물

HRID 869676노트

반응식

HRID 869676 반응식
[CH3:1][C:2]1[C:3]([C:12](=O)[CH2:13][C:14]#[N:15])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.O.[NH2:18][NH2:19].C(=O)(O)[O-].[Na+]>C(O)(=O)C.C(O)C.O>[CH3:1][C:2]1[C:3]([C:12]2[CH:13]=[C:14]([NH2:15])[NH:19][N:18]=2)=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2

참가 물질

7

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 516892Sodium BicarbonateHCID 67397893HCID 67397893, 화합물

생성물 1

HCID 178432134HCID 178432134, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A suspension of 3-(3-methylquinoxalin-2-yl)-3-oxopropanenitrile (45.8 g, 217 mmol) and hydrazine monohydrate (15.8 mL, 325 mmol) in acetic acid (109 mL) and ethanol (1083 mL) was refluxed for 17 h. After being cooled to ambient temperature, the reaction mixture was diluted with water (360 mL) and basified to pH 8 with sodium bicarbonate. The resulting precipitate was collected and washed with diisopropyl ether. The crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g), and then heated at 60° C. for 2 h. The precipitate was collected and washed with diisopropyl ether to give 3-(3-methylquinoxalin-2-yl)-1H-pyrazol-5-amine. MS (APCI): m/z 226 (M+H).

후처리

  1. temperaturewas refluxed for 17 h
  2. customThe resulting precipitate was collected
  3. washwashed with diisopropyl ether
  4. additionThe crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g)
  5. temperatureheated at 60° C. for 2 h
  6. customThe precipitate was collected
  7. washwashed with diisopropyl ether

출처 및 근거

ORD 기록
ord-3df8457ac8c84cd3ab0e48f7ef693f10
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969376B2

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