Hydrogen Peroxide → HCID 66701185、化合物

HRID 2062108ノート

反応式

HRID 2062108 の反応式
[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.O.P([O-])(O)(O)=[O:18].[Na+].OO.Cl([O-])=O.[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:18])=[O:15])[CH:3]=1

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 106320064-Fluoro-1-methoxy-2-naphthaldehydeHCID 23668197Sodium Chlorite

生成物 1

HCID 66701185HCID 66701185、化合物収率 280.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6342Acetonitrile溶媒

実験手順

9.3 g of 4-fluoro-1-methoxynaphthalene-2-carbaldehyde were dissolved in 100 mL of acetonitrile. 2.1 g sodium dihydrogenphosphate 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 dropwise 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.

後処理

  1. additionwere added dropwise
  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.

出典と根拠

ORDレコード
ord-9ebbb002d5bd49bfafd50ae006d3046d
出典データセット
uspto-grants-2012_10
特許番号
US08283479B2

反応ノート

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