Nitric Acid → 3-(2-Chloro-4-fluoro-5-nitrophenyl)-tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetic acid

HRID 725226

반응식

HRID 725226 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:14](=[O:15])[N:13]([CH3:16])[C:12](=[O:17])[N:11]([CH2:18][C:19]([O:21]C(C)C)=[O:20])[C:10]1=[O:25].[N+:26]([O-])([OH:28])=[O:27]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:26]([O-:28])=[O:27])=[CH:4][C:3]=1[N:9]1[C:14](=[O:15])[N:13]([CH3:16])[C:12](=[O:17])[N:11]([CH2:18][C:19]([OH:21])=[O:20])[C:10]1=[O:25]

참가 물질

4

반응물 2

HCID 944Nitric Acid4회HCID 57141938Isopropyl 3-(2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)acetate

생성물 1

HCID 540879253-(2-Chloro-4-fluoro-5-nitrophenyl)-tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetic acid

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of isopropyl 3-(2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate (48.7 g, 0.0508 mol) in concentrated sulfuric acid is cooled to 0° C., treated with 90% nitric acid (2.6 mL), stirred at room temperature overnight, treated with 90% nitric acid (1.0 mL), stirred for 4 hours, treated with 90% nitric acid (2.0 mL), stirred at room temperature overnight, treated with 90% nitric acid (1.0 mL), stirred for 1 hour and poured onto ice. The resultant aqueous solution is filtered to obtain a solid. A solution of the solid in ether is dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as a yellow foam which is identified by NMR spectral analyses.

후처리

  1. stirringstirred for 4 hours
  2. stirringstirred at room temperature overnight
  3. stirringstirred for 1 hour
  4. additionpoured onto ice
  5. filtrationThe resultant aqueous solution is filtered
  6. customto obtain a solid
  7. dry with materialA solution of the solid in ether is dried over anhydrous magnesium sulfate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b3f8b2cf0f734ee8a01d252540956db4
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705644

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