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

HRID 619885
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HRID 619885 반응식
[C:1](=[O:13])([O:11][CH3:12])[O:2][C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[Br:10].[N+:14]([O-])([OH:16])=[O:15]>S(=O)(=O)(O)O>[C:1](=[O:13])([O:11][CH3:12])[O:2][C:3]1[CH:8]=[C:7]([N+:14]([O-:16])=[O:15])[C:6]([F:9])=[CH:5][C:4]=1[Br:10]
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 92.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A rapidly stirred solution of 946 g (3.8 moles) of 2-bromo-4-fluorophenyl methyl carbonate in 1292 mL of sulfuric acid was cooled to 5°-10° C., and 368 g (4.18 moles) of 70% nitric acid was added dropwise over two hours. Upon complete addition, the reaction mixture was allowed to warm to ambient temperature and was stirred for two hours. The reaction mixture was poured into 5000 mL of ice water. Any material remaining in the reaction vessel was washed into the ice-water with 750 mL of water. The resultant solid was collected by filtration and washed with 1000 mL of water. The solid was dried with mild heat under reduced pressure to give 1031 g of 2-bromo-4-fluoro-5nitrophenyl methyl carbonate.

후처리

  1. additionUpon complete addition
  2. washwas washed into the ice-water with 750 mL of water
  3. filtrationThe resultant solid was collected by filtration
  4. washwashed with 1000 mL of water
  5. customThe solid was dried
  6. temperaturewith mild heat under reduced pressure

출처 및 근거

ORD 기록
ord-da56b96ee9b14929af58d018cd463f7a
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04818276

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