3-(5-Chloro-thiophen-2-ylmethoxy)-phthalic acid dimethyl ester → 3-(5-Chloro-thiophen-2-ylmethoxy)-phthalic acid

HRID 1690470ノート

反応式

HRID 1690470 の反応式
C[O:2][C:3](=[O:22])[C:4]1[C:5](=[C:10]([O:14][CH2:15][C:16]2[S:17][C:18]([Cl:21])=[CH:19][CH:20]=2)[CH:11]=[CH:12][CH:13]=1)[C:6]([O:8]C)=[O:7]>[OH-].[Na+]>[Cl:21][C:18]1[S:17][C:16]([CH2:15][O:14][C:10]2[CH:11]=[CH:12][CH:13]=[C:4]([C:3]([OH:22])=[O:2])[C:5]=2[C:6]([OH:8])=[O:7])=[CH:20][CH:19]=1

参加物

3

反応物 1

HCID 669061873-(5-Chloro-thiophen-2-ylmethoxy)-phthalic acid dimethyl ester

生成物 1

HCID 669067303-(5-Chloro-thiophen-2-ylmethoxy)-phthalic acid収率 76.4%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 3-(5-chloro-thiophen-2-ylmethoxy)-phthalic acid dimethyl ester (2.3 g, 6.7 mmol) in reagent alcohol (100 mL) and 3 N sodium hydroxide (60 mL) was refluxed for two hours. The solution was evaporated and the residue was dissolved in water (100 mL) and washed with methylene chloride (3×100 mL) then acidified to pH around 4. The resulting mixture was extracted with ethyl acetate (2×100 mL) and the combined organic layers was washed with water (2×100 mL), dried and concentrated to give 3-(5-chloro-thiophen-2-ylmethoxy)-phthalic acid as an off-white solid (1.6 g, 76% yield). The product was used in the next step without further purification.

後処理

  1. customThe solution was evaporated
  2. dissolutionthe residue was dissolved in water (100 mL)
  3. washwashed with methylene chloride (3×100 mL)
  4. extractionThe resulting mixture was extracted with ethyl acetate (2×100 mL)
  5. washthe combined organic layers was washed with water (2×100 mL)
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-0065bc287032480a98a624454989e9bd
出典データセット
uspto-grants-2012_04
特許番号
US08153659B2

反応ノート

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