Tetrahydrofuran → 4-Acetylthiomethyl-1,2,3-thiadiazole

HRID 1253115

반응식

HRID 1253115 반응식
CS(O[CH2:6][C:7]1[N:8]=[N:9][S:10][CH:11]=1)(=O)=O.[S:12]1C=CC=C1CC([O-])=O.[Na+].[O:22]1CC[CH2:24][CH2:23]1>CCOCC>[C:23]([S:12][CH2:6][C:7]1[N:8]=[N:9][S:10][CH:11]=1)(=[O:22])[CH3:24]

참가 물질

5

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온도
23 °C

실험 절차

To a solution of 1,2,3-thiadiazol-4-ylmethanol methanesulfonate (0.90 g, 4.6 mmol) in tetrahydrofuran (9 mL) was added an aqueous solution (2 mL) of sodium thiolacetate [prepared from thiolacetic acid (0.38 mL, 5.3 mmol) and sodium bicarbonate (0.445 g, 5.3 mmol)]. The resulting mixture was stirred at 23° C. for 1 h and diluted with ether (75 mL). The organic solution was washed with water (3×3 mL), dried (MgSO4) and concentrated. The crude mixture was purified by chromatography (silica gel column: 1.4×19 cm) with 50% ether in hexane as eluting solvent to give 0.60 g (75%);

후처리

  1. washThe organic solution was washed with water (3×3 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customThe crude mixture was purified by chromatography (silica gel column: 1.4×19 cm) with 50% ether in hexane
  5. washas eluting solvent
  6. customto give 0.60 g (75%)

출처 및 근거

ORD 기록
ord-c15658dc0d6640a38043aece635bc8ab
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04746736

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