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Nitric Acid → HCID 19377779, 화합물

HRID 1768759
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반응식

HRID 1768759 반응식
[O:1]1[CH:5]=[CH:4][C:3]([NH:6][C:7]2[CH:8]=[C:9]3[CH2:17][O:16][CH2:15][CH2:14][C:10]3=[N+:11]([O-:13])[CH:12]=2)=[N:2]1.C(Cl)(Cl)Cl.[N+:22]([O-])([OH:24])=[O:23]>>[O:1]1[CH:5]=[CH:4][C:3]([NH:6][C:7]2[C:8]([N+:22]([O-:24])=[O:23])=[C:9]3[CH2:17][O:16][CH2:15][CH2:14][C:10]3=[N+:11]([O-:13])[CH:12]=2)=[N:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 6212ChloroformHCID 19377768HCID 19377768, 화합물

생성물 1

HCID 19377779HCID 19377779, 화합물수율 70%

반응 조건

온도
55 °C

실험 절차

A solution of 653 mg of Compound 5 obtained in the above step (1) as crystals in 3.2 ml of fuming nitric acid is stirred at 55° C. for 3 hours. The reaction mixture is chilled, poured onto ice water and shaken with chloroform. The extract is washed with water, aqueous disodium hydrogen phosphate and saturated saline in this order, dried over anhydrous magnesium sulfate and concentrated to remove the solvent. The resultant residue is washed with methanol to give 551 mg of the titled compound 6 as light yellow crystals.

후처리

  1. temperatureThe reaction mixture is chilled
  2. additionpoured onto ice water
  3. washThe extract is washed with water, aqueous disodium hydrogen phosphate and saturated saline in this order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customto remove the solvent
  7. washThe resultant residue is washed with methanol

출처 및 근거

ORD 기록
ord-89404e43642b41fab713533135bf6905
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05378848

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