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Nitric Acid → 5-Chloro-3-methyl-4-nitro-1-phenyl-1H-pyrazole

HRID 2398616
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인쇄 미리보기

반응식

HRID 2398616 반응식
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([CH3:13])[CH:3]=1.[N+:14]([O-])([O:16]C(=O)C)=[O:15].[N+]([O-])(O)=O>C(OC(=O)C)(=O)C>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([CH3:13])[C:3]=1[N+:14]([O-:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 11557Acetyl nitrateHCID 27357715-Chloro-3-methyl-1-phenyl-1H-pyrazole

생성물 1

HCID 8493605-Chloro-3-methyl-4-nitro-1-phenyl-1H-pyrazole

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매2회

실험 절차

A solution of 9.6 g (0.05 mole) of 5-chloro-3-methyl-1-phenylpyrazole and 25 ml of acetic anhydride was added at 10° C. to a solution of acetyl nitrate prepared from 25 ml of 90% nitric acid and 10 ml of acetic anhydride. The solution was stirred 2 hours at 20°-30° C. and carefully poured onto ice water. The solid was filtered off and washed with cold water. One recrystallization from ethanol gave long white needles of product.

후처리

  1. additioncarefully poured onto ice water
  2. filtrationThe solid was filtered off
  3. washwashed with cold water
  4. customOne recrystallization from ethanol
  5. customgave long white needles of product

출처 및 근거

ORD 기록
ord-d251477fdf9343c9a39124ad7f8c03a8
출처 데이터셋
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04025530

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