Sodium Hydroxide → 2-Thioanisylterepthalic acid

HRID 1885380

반응식

HRID 1885380 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:19]=[C:18]([C:20]([O:22]C)=[O:21])[CH:17]=[CH:16][C:11]=1[C:12]([O:14]C)=[O:13].[OH-].[Na+]>CO>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[CH:16][C:11]=1[C:12]([OH:14])=[O:13]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86744855Dimethyl 2-thioanisylterepthalate

생성물 1

HCID 867448562-Thioanisylterepthalic acid수율 76.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Dimethyl 2-thioanisylterepthalate (3.92 g) was suspended in methanol (45.9 ml), 5M NaOH (13.5 ml) was added. The reaction mixture was heated at reflux for 1.5 hours. The methanol was removed under reduced pressure. The residue was treated with ethyl acetate and water and the layers separated. The aqueous layer was washed once with ethyl acetate. The aqueous layer was then acidified with 2N HCl and extracted three times with ethyl acetate. These combined organic extracts were then dried over MgSO4, filtered and evaporated under reduced pressure gave the product (2.75 g).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. customThe methanol was removed under reduced pressure
  4. additionThe residue was treated with ethyl acetate and water
  5. customthe layers separated
  6. washThe aqueous layer was washed once with ethyl acetate
  7. extractionextracted three times with ethyl acetate
  8. dry with materialThese combined organic extracts were then dried over MgSO4
  9. filtrationfiltered
  10. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-325ac8452fac4a5c96e60f9b3bb1bdce
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05144028

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