Hydrochloric Acid → HCID 59326505、化合物

HRID 1929560ノート

反応式

HRID 1929560 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:14]=[C:13]([O:15]C(=O)C)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:19])[CH:11]=2)[CH:6]=1)=[O:4].C[O-].[Na+].Cl>CO>[CH3:1][O:2][C:3]([C:5]1[CH:14]=[C:13]([OH:15])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:19])[CH:11]=2)[CH:6]=1)=[O:4]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 593266124-Acetoxy-6-fluoro-naphthalene-2-carboxylic acid methyl ester

生成物 1

HCID 59326505HCID 59326505、化合物収率 107.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4-acetoxy-6-fluoro-naphthalene-2-carboxylic acid methyl ester (1 g, 3.8 mmol) in methanol (20 mL) was added sodium methoxide (309 mg, 5.7 mmol). After being stirred at room temperature for 1 hour, the reaction mixture was acidified to pH 3 with 1N hydrochloric acid. The resulting precipitate was collected by filtration and dissolved in ethyl acetate. The organic solution was dried over sodium sulfate, and concentrated in vacuo to afford 900 mg of crude 6-fluoro-4-hydroxy-naphthalene-2-carboxylic acid methyl ester as a pale yellow solid, which was used in the next step without further purification.

後処理

  1. filtrationThe resulting precipitate was collected by filtration
  2. dissolutiondissolved in ethyl acetate
  3. dry with materialThe organic solution was dried over sodium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-56eea3f0c2d34aad9e65fddf6d057edd
出典データセット
uspto-grants-2012_05
特許番号
US08188090B2

反応ノート

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