Acetone → HCID 58957422, 화합물

HRID 2075297노트

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HRID 2075297 반응식
[CH3:1][C:2]([CH3:4])=O.[CH2:5]([N:8]1[C:12](=[O:13])[CH2:11][NH:10][C:9]1=[S:14])[CH:6]=[CH2:7].N1CCOCC1>C(OCC)(=O)C>[CH2:5]([N:8]1[C:12](=[O:13])[C:11](=[C:2]([CH3:4])[CH3:1])[NH:10][C:9]1=[S:14])[CH:6]=[CH2:7]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 8083MorpholineHCID 3032418Hydantoin, 3-allyl-2-thioxo-

생성물 1

HCID 58957422HCID 58957422, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A flask equipped with a reflux condenser and nitrogen atmosphere was charged with acetone (20 mL), 3-allylthiohydantoin (2.0 g, 0.013 mol), and morpholine (1.1 g, 0.013 mol). The mixture was heated at reflux for 80 min and, after cooling, was diluted with 40 mL of ethyl acetate. The resulting solution was washed with 2×20 mL 1.2 M HCl, 20 mL of water, and 20 mL of saturated aqueous NaCl. The solution was then filtered through 1 PS paper and concentrated to dryness at aspirator pressure and then high vacuum. The off-white crystalline residue weighed 2.3 g (92%). No other components were detectable by HPLC at 215 nm. NMR (CDCl3) δ 9.9 (bs, 1H), 5.1-6.1 (m, 3H), 4.6 (d, 2H), 2.3 (s, 3H), 2.0 (s, 3H).

후처리

  1. customA flask equipped with a reflux condenser
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 80 min
  4. temperatureafter cooling
  5. washThe resulting solution was washed with 2×20 mL 1.2 M HCl, 20 mL of water, and 20 mL of saturated aqueous NaCl
  6. filtrationThe solution was then filtered through 1 PS paper
  7. concentrationconcentrated to dryness at aspirator pressure

출처 및 근거

ORD 기록
ord-9b2fa6d0c8084e05acf8e68658048d59
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919630B2

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