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

HRID 1024354

반응식

HRID 1024354 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-92c5b61e2c3a4d50b6f5137860c46781
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722887B2

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