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Acetic Acid → 2,4,6,7-Tetramethyl-benzo[1,3]oxathiol-5-ol

HRID 2308855
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HRID 2308855 반응식
C([O:4][C:5]1[C:6]([CH3:17])=[C:7]([CH3:16])[C:8]2[O:12][CH:11]([CH3:13])[S:10][C:9]=2[C:14]=1[CH3:15])(=O)C.C[O-].[Na+].O.C(O)(=O)C>CO>[OH:4][C:5]1[C:6]([CH3:17])=[C:7]([CH3:16])[C:8]2[O:12][CH:11]([CH3:13])[S:10][C:9]=2[C:14]=1[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 10942334Sodium MethoxideHCID 13592035HCID 13592035, 화합물

생성물 1

HCID 135920402,4,6,7-Tetramethyl-benzo[1,3]oxathiol-5-ol수율 82.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2.9 g of 5-acetoxy-2,4,6,7-tetramethyl-1,3-benzoxathiole, prepared as described in Example 22, were dissolved in 30 ml of methanol, 1.3 g of sodium methoxide was added to the solution, and the mixture was allowed to react at room temperature for 3 hours. At the end of this time, the reaction mixture was poured into water and the solution was neutralized by adding acetic acid. The separated product was extracted with benzene and the extract was washed with water and dried over anhydrous sodium sulfate. The solvent was evaporated off. The crude product thus obtained was purified by silica gel column chromatography. From the fraction eluted with a 1:1 by volume mixture of hexane and benzene were obtained 2.0 g of the title compound, melting at 125°-127° C.

후처리

  1. customto react at room temperature for 3 hours
  2. extractionThe separated product was extracted with benzene
  3. washthe extract was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated off
  6. customThe crude product thus obtained
  7. customwas purified by silica gel column chromatography
  8. washFrom the fraction eluted with a 1:1 by volume mixture of hexane

출처 및 근거

ORD 기록
ord-642fb35839614a1c8027829d1657d6cd
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04691027

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