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Ethyl 5-methoxy-4-((1-methylpiperidin-4-yl)methoxy)-2-nitrobenzoate → Ethyl 2-amino-5-methoxy-4-((1-methylpiperidin-4-yl)methoxy)benzoate

HRID 454015
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HRID 454015 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([N+:23]([O-])=O)=[CH:12][C:13]=1[O:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]1)[C:6]([O:8][CH2:9][CH3:10])=[O:7].[H][H]>CO.[Pt]>[NH2:23][C:11]1[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]([O:2][CH3:1])=[C:13]([O:14][CH2:15][CH:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)[CH:12]=1
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참가 물질

5

반응물 2

HCID 21874808Ethyl 5-methoxy-4-((1-methylpiperidin-4-yl)methoxy)-2-nitrobenzoateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 21874813Ethyl 2-amino-5-methoxy-4-((1-methylpiperidin-4-yl)methoxy)benzoate수율 80%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 887Methanol용매

실험 절차

A suspension of ethyl 3-methoxy-4-(1-methylpiperidin-4-ylmethoxy)-6-nitrobenzoate (3.89 g, 10 mmol) in methanol (80 ml) containing 10% platinum on activated carbon (50% wet) (389 mg) was hydrogenated at 1.8 atmospheres pressure until uptake of hydrogen ceased. The mixture was filtered and the filtrate was evaporated. The residue was dissolved in water (30 ml) and adjusted to pH10 with a saturated solution of sodium hydrogen carbonate. The mixture was diluted with ethyl acetate/ether (1/1) and the organic layer was separated. The aqueous layer was further extracted with ethyl acetate/ether and the organic layers were combined. The organic layers were washed with water, brine, dried (MgSO4), filtered and evaporated. The resulting solid was triturated in a mixture of ether/petroleum ether, filtered, washed with petroleum ether and dried under vacuum at 60° C. to give ethyl 6-amino-3-methoxy-4-(1-methylpiperidin-4-ylmethoxy)benzoate (2.58 g, 80%).

후처리

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated
  3. dissolutionThe residue was dissolved in water (30 ml)
  4. additionThe mixture was diluted with ethyl acetate/ether (1/1)
  5. customthe organic layer was separated
  6. extractionThe aqueous layer was further extracted with ethyl acetate/ether
  7. washThe organic layers were washed with water, brine
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. customevaporated
  11. customThe resulting solid was triturated in a mixture of ether/petroleum ether
  12. filtrationfiltered
  13. washwashed with petroleum ether
  14. customdried under vacuum at 60° C.

출처 및 근거

ORD 기록
ord-3fc337d18cb94eb5ac4ff9eb0652ea8a
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08492560B2

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