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

HRID 1915175노트

반응식

HRID 1915175 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5bbe4dce9ea24d25829c76d4bc068bde
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614328B2

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