1,4-Dioxane → HCID 21914731, 화합물

HRID 2117867노트

반응식

HRID 2117867 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1.[O:14]1CCOCC1>O>[OH:14][CH2:2][C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1

참가 물질

4

반응물 2

HCID 312751,4-DioxaneHCID 21914836Ethyl [4-(chloromethyl)-1,3-thiazol-2-yl]carbamate

생성물 1

HCID 21914731HCID 21914731, 화합물수율 98.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixed solution of ethyl 4-(chloromethyl)-1,3-thiazol-2-ylcarbamate (500 mg) in 1,4-dioxane (5 ml) and water (10 ml) was refluxed with stirring for 3.5 hours. After cooling, it was concentrated under reduced pressure. The mixture was partitioned between ethyl acetate and water. The organic phase was separated, washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (10 g) using a mixed solvent of hexane and ethyl acetate (2:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give colorless syrup (450 mg, 98.2%).

후처리

  1. temperatureAfter cooling
  2. concentrationit was concentrated under reduced pressure
  3. customThe mixture was partitioned between ethyl acetate and water
  4. customThe organic phase was separated
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography on silica gel (10 g)
  9. additionThe fractions containing the objective compound
  10. customwere collected
  11. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-e711d4cf4c1b41f2aaaa89aa6168e0eb
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07442715B2

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