Nitric Acid → 4,6-Dihydroxy-5-nitro-2-trifluoromethyl-nicotinic acid ethyl ester

HRID 639705노트

반응식

HRID 639705 반응식
[CH2:1]([O:3][C:4](=[O:17])[C:5]1[C:10]([OH:11])=[CH:9][C:8]([OH:12])=[N:7][C:6]=1[C:13]([F:16])([F:15])[F:14])[CH3:2].[N+:18]([O-])([OH:20])=[O:19]>S(=O)(=O)(O)O>[CH2:1]([O:3][C:4](=[O:17])[C:5]1[C:10]([OH:11])=[C:9]([N+:18]([O-:20])=[O:19])[C:8]([OH:12])=[N:7][C:6]=1[C:13]([F:14])([F:15])[F:16])[CH3:2]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 178470040HCID 178470040, 화합물

생성물 1

HCID 1784691454,6-Dihydroxy-5-nitro-2-trifluoromethyl-nicotinic acid ethyl ester

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

4,6-dihydroxy-2-trifluoromethyl-nicotinic acid ethyl ester (1 g, 3.9 mmol) was dissolved in 10 mL of concentrated sulfuric acid and 2 mL of fuming nitric acid was added dropwise at room temperature. Once the addition was complete, the mixture was stirred at room temperature for 30 minutes. The mixture was then poured into crushed ice and the white precipitate was collected, dissolved in 50 mL of ethyl acetate, washed with 50 mL of water and 50 mL of brine, dried over magnesium sulfate and the solvent was removed in vacuo to give 1.1 g of the title compound as a white solid.

후처리

  1. additionOnce the addition
  2. additionThe mixture was then poured
  3. custominto crushed ice
  4. customthe white precipitate was collected
  5. dissolutiondissolved in 50 mL of ethyl acetate
  6. washwashed with 50 mL of water and 50 mL of brine
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-60eb538ffc4545fc80187be09bb4af56
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691877B2

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