HCID 21914731, 화합물 → HCID 21914837, 화합물

HRID 1246458노트

반응식

HRID 1246458 반응식
[OH:1][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>C(Cl)(Cl)Cl.CO.[O-2].[Mn+4].[O-2]>[CH: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:1]

참가 물질

5

반응물 1

HCID 21914731HCID 21914731, 화합물

생성물 1

HCID 21914837HCID 21914837, 화합물수율 106.4%

시약·촉매·용매 3

HCID 178418406HCID 178418406, 화합물촉매2회HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

To a mixed solution of ethyl 4-(hydroxymethyl)-1,3-thiazol-2-ylcarbamate (446 mg) in chloroform (30 ml) and methanol (3 ml) was added portionwise manganese (IV) oxide chemicals treated (1.92 g) at room temperature. After the mixture was stirred at the same temperature for 2 hours, then treated manganese (IV) oxide chemicals (250 mg) was added again to the solution, and it was stirred at 50° C. for 3 hours. Manganese (IV) oxide was removed by filtration and the filtrate was 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 (4:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give colorless powder (470 mg, 106.4%).

후처리

  1. additiontreated (1.92 g) at room temperature
  2. stirringwas stirred at 50° C. for 3 hours
  3. customManganese (IV) oxide was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (10 g)
  6. additionThe fractions containing the objective compound
  7. customwere collected
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d99145b84e0344b8b2e4497e0b87da62
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07125901B2

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