Hydrazine hydrate (1:1) → 3-Hydrazino-6-phenyl-1,2,4-triazine

HRID 1099032노트

반응식

HRID 1099032 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[NH:2]([C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1)[NH2:3]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 110306323-Chloro-6-phenyl-1,2,4-triazine

생성물 1

HCID 64051603-Hydrazino-6-phenyl-1,2,4-triazine수율 93%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
0 °C

실험 절차

Hydrazine hydrate (1.50 mL, 0.0308 mol) was added to suspension of 3-chloro-6-phenyl-1,2,4-triazine (2.20 g, 0.0115 mol) in pyridine (12.0 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 formed was collected and dried under high vacuum to give the desired product (2.0 g, 93%). Analytical LCMS: (M+H)+=188.1.

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 formed
  8. customwas collected
  9. customdried under high vacuum

출처 및 근거

ORD 기록
ord-1fe9dd1f9bb44cd9b77e5baa16aa9e03
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143251B2

반응 노트

불러오는 중…