Sodium Hydroxide → 3-(4-Chlorophenyl)-4,5-dihydro-1H-pyrazole

HRID 12493

반응식

HRID 12493 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH2:10][CH2:11][N:12](C)C)=[CH:5][CH:4]=1.O.[NH2:17]N.[OH-].[Na+]>CO>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:10][CH2:11][NH:12][N:17]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 2003701-Propanone, 1-(4-chlorophenyl)-3-(dimethylamino)-, hydrochloride (1:1)

생성물 1

HCID 131437003-(4-Chlorophenyl)-4,5-dihydro-1H-pyrazole

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
50 °C

실험 절차

Under N2 atmosphere, 1-(4-chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride (37.2 g) was dissolved in warm MeOH (75 mL), and slowly added to a solution of hydrazine hydrate (23 mL) and 50% aqueous NaOH (12 mL) in MeOH (30 mL) stirred at 50° C. The mixture was refluxed for 2 hours, and evaporated under reduced pressure. Water was added to the residue, followed by extraction with DCM. The organic phase was washed twice with water, dried and evaporated under reduced pressure, to give 25.0 g of a yellow solid, m.p. 90-100° C.

후처리

  1. temperatureThe mixture was refluxed for 2 hours
  2. customevaporated under reduced pressure
  3. additionWater was added to the residue
  4. extractionfollowed by extraction with DCM
  5. washThe organic phase was washed twice with water
  6. customdried
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-46422b9f44604933bc9aea30a17a0796
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728018B2

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