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Hydrochloric Acid → HCID 57621407, 화합물

HRID 490554
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HRID 490554 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][NH:8][C:7]2=[O:13])([O-:3])=[O:2].[CH2:14](Br)[CH:15]=[CH2:16].[OH-].[Na+].Cl>O.[OH-].[K+]>[CH2:16]([N:9]1[C:10]2[C:6](=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=2)[C:7](=[O:13])[NH:8]1)[CH:15]=[CH2:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7841Allyl bromide2회HCID 14798Sodium HydroxideHCID 53746612,3-Dihydro-5-nitro-1H-indazol-3-one

생성물 1

HCID 57621407HCID 57621407, 화합물수율 66.6%

시약·촉매·용매 2

HCID 962Water용매
HCID 14797
Potassium Hydroxide
용매

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온도
77.5 °C

실험 절차

5-Nitro-1,2-dihydro-indazol-3-one (prepared according to Org. Synth. 1949, 29, 54 or Chem Ber. 1942, 75, 1104) (9.36 g) was suspended in 40 ml water and 57.5 ml 1N KOH. Allyl bromide (6.32 g) was added in one portion. The mixture was stirred at 75-80° C. for 1.5 hours. Then NaOH (15%, 5 mL) and allyl bromide (1 g) was added. The reaction mixture was stirred for a further 30 min. The mixture was neutralized with 3N HCl at <10° C. and filtered. The solid was washed with water and dried. The solid was then suspended in 10 ml ethyl acetate and stirred at ambient temperature for 3 hours, then filtered and dried to afford the desired 1-allyl-5-nitro-1,2-dihydro-indazol-3-one (7.63 g) as a yellow solid.

후처리

  1. stirringThe reaction mixture was stirred for a further 30 min
  2. filtrationfiltered
  3. washThe solid was washed with water
  4. customdried
  5. stirringstirred at ambient temperature for 3 hours
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-24d3449e796d4b4ca8df8581710e5e74
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528158B2

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