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Methyl iodide → HCID 178503574, 화합물

HRID 324478
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HRID 324478 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17](=[S:23])[NH:18][C:19](=[O:22])[NH:20][CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:24]=1.[C:25](=O)(O)[O-].[Na+].CI>C(O)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17]([S:23][CH3:25])=[N:18][C:19](=[O:22])[NH:20][CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6328Methyl iodide2회HCID 516892Sodium BicarbonateHCID 88152155HCID 88152155, 화합물

생성물 1

HCID 178503574HCID 178503574, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

A suspension of the product from example 38, step (v) (1.8 g) in ethanol (200 ml) and sodium bicarbonate (0.5 g) in water (15 ml) was heated until a complete solution formed. After cooling to room temperature methyl iodide (0.33 ml) was added and the whole stirred for 18 h. Another aliquot of methyl iodide was added (0.2 ml) followed by heating at 50° C. for 4 h. The reaction mixture was concentrated under reduced pressure and then partitioned between dichloromethane and brine. The organic phase was collected, dried (MgSO4) and evaporated under reduced pressure to leave a beige foam. Purification was by chromatography eluting with ethyl acetate/methanol mixtures to give the subtitle product as colourless solid.

후처리

  1. temperaturewas heated until a complete solution
  2. customformed
  3. additionwas added
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. custompartitioned between dichloromethane and brine
  6. customThe organic phase was collected
  7. dry with materialdried (MgSO4)
  8. customevaporated under reduced pressure
  9. customto leave a beige foam
  10. customPurification
  11. washeluting with ethyl acetate/methanol

출처 및 근거

ORD 기록
ord-ce7066069a78420da825cc22f47f2410
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218376B1

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