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Nitric Acid → Methyl 2-bromo-4-fluoro-5-nitrophenoxyformate

HRID 48492
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반응식

HRID 48492 반응식
[Br:1][C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[O:4][C:5]([O:7][CH3:8])=[O:6].[N+:14]([O-])([OH:16])=[O:15]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:12]=[C:11]([F:13])[C:10]([N+:14]([O-:16])=[O:15])=[CH:9][C:3]=1[O:4][C:5]([O:7][CH3:8])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 13268177Carbonic acid, 2-bromo-4-fluorophenyl methyl ester

생성물 1

HCID 13268178Methyl 2-bromo-4-fluoro-5-nitrophenoxyformate수율 97.7%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

Then, 110 g (0.44 mol) of methyl 2-bromo-4-fluorophenoxyformate was dissolved in 250 ml of sulfuric acid, to which a mixed acid of 30 g of fuming nitric acid and 30 ml of sulfuric acid was added dropwise at 5° C. or lower, and the mixture was stirred for 2 hours. The reaction mixture was poured onto ice, and the precipitated crystals were collected by filtration, washed with water, and dried, which afforded 126 g (0.43 mol) of methyl 2-bromo-4-fluoro-5-nitrophenoxyformate.

후처리

  1. additionwas added dropwise at 5° C.
  2. additionThe reaction mixture was poured onto ice
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-0f13797f74d449c092f060ea899a8952
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06703503B2

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