Hydrazine hydrate (1:1) → 6-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazine

HRID 1099034노트

반응식

HRID 1099034 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[F:17][C:14]1[CH:15]=[CH:16][C:11]([C:8]2[N:7]=[N:6][C:5]([NH:2][NH2:3])=[N:10][CH:9]=2)=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 213152193-Chloro-6-(4-fluorophenyl)-1,2,4-triazine

생성물 1

HCID 213152186-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazine수율 91.9%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
0 °C

실험 절차

Hydrazine hydrate (0.28 mL, 0.0057 mol) was added to a suspension of 3-chloro-6-(4-fluorophenyl)-1,2,4-triazine (400 mg, 0.002 mol) in pyridine (4 mL) at 0° C. and stirred at 0° C. until a precipitate formed. The mixture was then heated at 65° C. for 30 min. The solvent was evaporated under reduced pressure. The residue was triturated with water, filtered, and washed with water. The crystalline solid was collected and dried under high vacuum to give the desired product (360 mg, 91.9%). Analytical LCMS: (M+H)+=206.1.

후처리

  1. customformed
  2. temperatureThe mixture was then heated at 65° C. for 30 min
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was triturated with water
  5. filtrationfiltered
  6. washwashed with water
  7. customThe crystalline solid was collected
  8. customdried under high vacuum

출처 및 근거

ORD 기록
ord-9108564c25fe4982a19aeebc9494f256
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143251B2

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