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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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p-Toluenesulfonic acid → 1-{[4-(2,3-Dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyrid-2-yl]methoxy}-2-hydroxy-2-methyl-3-(1,2,4-triazol-4-yl)propane

HRID 329687
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HRID 329687 반응식
[NH2:1][CH2:2][C:3]([OH:32])([CH3:31])[CH2:4][O:5][CH2:6][C:7]1[NH:8][C:9]([CH3:30])=[C:10]([C:26]([O:28][CH3:29])=[O:27])[CH:11]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[C:19]=2[Cl:25])[C:12]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14].CN(C)/[CH:35]=[N:36]/[N:37]=[CH:38]/N(C)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[Cl:25][C:19]1[C:20]([Cl:24])=[CH:21][CH:22]=[CH:23][C:18]=1[CH:11]1[C:10]([C:26]([O:28][CH3:29])=[O:27])=[C:9]([CH3:30])[NH:8][C:7]([CH2:6][O:5][CH2:4][C:3]([OH:32])([CH3:31])[CH2:2][N:1]2[CH:38]=[N:37][N:36]=[CH:35]2)=[C:12]1[C:13]([O:15][CH2:16][CH3:17])=[O:14]
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참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 9613942N'-((Dimethylamino)methylene)-N,N-dimethylformohydrazonamideHCID 148106031-Amino-3-{[4-(2,3-dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyrid-2-yl]methoxy}-2-hydroxy-2-methylpropane

생성물 1

HCID 148106011-{[4-(2,3-Dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyrid-2-yl]methoxy}-2-hydroxy-2-methyl-3-(1,2,4-triazol-4-yl)propane수율 65.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 1-amino-3-{[4-(2,3-dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyrid-2-yl]methoxy}-2-hydroxy-2-methylpropane (0.25 g), N,N-dimethylformamide azine (0.21 g) and para-toluenesulphonic acid (10 mg) in toluene (10 ml) was heated under reflux for 1.5 hours and then partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water, dried over Na2SO4 and evaporated. The residue was purified by chromatography on SiO2 (5 g) using dichloromethane plus 0-5% methanol as the eluant. Appropriate fractions were combined and evaporated and the residue triturated with ether. The resulting solid was collected, washed with ether and dried to give the title compound (0.18 g), m.p. 172°-176° C.

후처리

  1. temperatureunder reflux for 1.5 hours
  2. custompartitioned between ethyl acetate and water
  3. customThe layers were separated
  4. washthe organic layer was washed with water
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customThe residue was purified by chromatography on SiO2 (5 g)
  8. customevaporated
  9. customthe residue triturated with ether
  10. customThe resulting solid was collected
  11. washwashed with ether
  12. customdried

출처 및 근거

ORD 기록
ord-170082e21d3b450ba35f06bc88b5aae8
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04892881

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