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Methyl iodide → HCID 5282538, 화합물

HRID 567889
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HRID 567889 반응식
[O-]CC.[Na+].[C:5]([NH:8][C:9](=[O:36])[N:10]([CH2:32][CH:33]([CH3:35])[CH3:34])[C:11]1[S:12][C:13]([CH2:21][C:22]2[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[CH:25]=[CH:24][CH:23]=2)=[CH:14][C:15]=1[C:16]([O:18]CC)=O)(=O)C.IC>C(O)C>[CH3:5][N:8]1[C:16](=[O:18])[C:15]2[CH:14]=[C:13]([CH2:21][C:22]3[C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[CH:25]=[CH:24][CH:23]=3)[S:12][C:11]=2[N:10]([CH2:32][CH:33]([CH3:34])[CH3:35])[C:9]1=[O:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 2723922Sodium ethoxideHCID 5282537HCID 5282537, 화합물

생성물 1

HCID 5282538HCID 5282538, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium ethoxide (0.18 g) was added to a stirred solution of N′-acetyl-N-(2-methylpropyl)-N-[3-ethoxycarbonyl-5-(1-naphthalenylmethyl)-2-thienyl]urea (Example 3, step c), 0.30 g) in ethanol (6 ml). After 6 hours, iodomethane (0.165 ml) was added. After a further 16 hours iodomethane (0.165 ml) was added, After a further 24 hours, the reaction mixture was poured onto hydrochloric acid (2M, 30 ml) and extracted with ethyl acetate (2×30 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography over silica, eluting with ether:hexane (1:1) and then triturated with ether to give the title compound (0.24 g).

후처리

  1. additionthe reaction mixture was poured onto hydrochloric acid (2M, 30 ml)
  2. extractionextracted with ethyl acetate (2×30 ml)
  3. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography over silica
  7. washeluting with ether:hexane (1:1)
  8. customtriturated with ether

출처 및 근거

ORD 기록
ord-46391c2a17f640b5adcf6d2396d0c153
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06180635B2

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