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Hydrochloric Acid → Methyl 4-{[cyclohexyl(2-ethyl-5-formylthiophen-3-yl)methyl]amino}benzoate

HRID 1877258
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HRID 1877258 반응식
Cl[CH:2]([CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[C:3]1[CH:4]=[C:5]([CH:10]2[O:14]CCO2)[S:6][C:7]=1[CH2:8][CH3:9].[NH2:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=1.[I-].[Na+].Cl>O1CCCC1.O.CN(C)C(=O)C>[CH:15]1([CH:2]([NH:21][C:22]2[CH:23]=[CH:24][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:30][CH:31]=2)[C:3]2[CH:4]=[C:5]([CH:10]=[O:14])[S:6][C:7]=2[CH2:8][CH3:9])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]1
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 12082Methyl 4-aminobenzoateHCID 685143042-{4-[Chloro(cyclohexyl)methyl]-5-ethylthiophen-2-yl}-1,3-dioxolane

생성물 1

HCID 86646397Methyl 4-{[cyclohexyl(2-ethyl-5-formylthiophen-3-yl)methyl]amino}benzoate수율 54.4%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매
HCID 31374Dimethylacetamide용매

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온도
100 °C

실험 절차

To a mixture of 2-{4-[chloro(cyclohexyl)methyl]-5-ethylthiophen-2-yl}-1,3-dioxolane (3.08 g) synthesized above, methyl 4-aminobenzoate (2.96 g), sodium iodide (2.98 g) and N,N-dimethylacetamide (60 mL) sodium carbonate (2.08 g) was added, and the mixture was stirred overnight at 100° C. under an argon atmosphere. Water was added to quench the reaction, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (30% ethyl acetate/hexane) to give a yellow oil. To a solution of the obtained oil in tetrahydrofuran (40 mL) was added 1N hydrochloric acid (10 mL), and the mixture was stirred at room temperature for 1 hr. Tetrahydrofuran was evaporated using evaporator, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (40% ethyl acetate/hexane) to give the title compound (2.05 g, 54%) as a yellow solid.

후처리

  1. additionwas added
  2. customto quench
  3. customthe reaction
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (30% ethyl acetate/hexane)
  9. customto give a yellow oil
  10. stirringthe mixture was stirred at room temperature for 1 hr
  11. customTetrahydrofuran was evaporated
  12. customevaporator
  13. extractionthe mixture was extracted with ethyl acetate
  14. washThe extract was washed with saturated brine
  15. dry with materialdried over magnesium sulfate
  16. concentrationconcentrated under reduced pressure
  17. customThe residue was purified by silica gel column chromatography (40% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-8e66bf3891d14783b87fbceec6277897
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309580B2

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