Hydrogen Peroxide → HCID 66701185, 화합물

HRID 1039117노트

반응식

HRID 1039117 반응식
[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH3:13])=[C:4]([CH:14]=[O:15])[CH:3]=1.[Na].OO.Cl([O-])=[O:20].[Na+]>C(#N)C.O>[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH3:13])=[C:4]([C:14]([OH:20])=[O:15])[CH:3]=1

참가 물질

7

반응물 4

HCID 784Hydrogen PeroxideHCID 5360545SodiumHCID 106320064-Fluoro-1-methoxy-2-naphthaldehydeHCID 23668197Sodium Chlorite

생성물 1

HCID 66701185HCID 66701185, 화합물수율 93.7%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6342Acetonitrile용매

실험 절차

9.3 g of 4-fluoro-1-methoxynaphthalene-2-carbaldehyde were dissolved in 100 ml of acetonitrile. 2.1 g sodium dihydrogenphsophate monohydrate in 10 ml of water were added, followed by the addition of 9.5 ml hydrogen peroxide (30%). 8.9 g sodium chlorite, dissolved in 20 ml water were added drop wise while maintaining an internal temperature between 5° C. and 15° C. The reaction was then allowed to come to room temp over 2.5 h. The precipitated solid was filtered with suction, and the solid was washed with water, and dried in vacuo at 40° C. to yield 9.4 g of 4-fluoro-1-methoxynaphthalene-2-carboxylic acid. The filtrate was treated with 60 ml of cold 10% aqueous sodium bisulfite solution. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with water and brine. The organic layer was washed with 0.2 N NaOH twice. The washes were acidified with 6 N HCl to pH 3, whereupon crystallization occurred. The precipitating product was filtered, washed with water and dried in vacuo at 40° C. to yield a second batch of 1.0 g of 4-fluoro-1-methoxynaphthalene-2-carboxylic acid.

후처리

  1. additionwere added drop wise
  2. temperaturewhile maintaining an internal temperature between 5° C. and 15° C
  3. filtrationThe precipitated solid was filtered with suction
  4. washthe solid was washed with water
  5. customdried in vacuo at 40° C.

출처 및 근거

ORD 기록
ord-fd95d4e764c049ec8e018328dc1237a7
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552033B2

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