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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 18542632, 화합물 → HCID 18542720, 화합물

HRID 1268230
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인쇄 미리보기

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HRID 1268230 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[C:24]([C:25]([O:27]C)=[O:26])=[CH:23][C:22]([N+:29]([O-:31])=[O:30])=[CH:21][C:16]=2[C:17]([O:19]C)=[O:18])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>Cl>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([O:14][C:15]2[C:24]([C:25]([OH:27])=[O:26])=[CH:23][C:22]([N+:29]([O-:31])=[O:30])=[CH:21][C:16]=2[C:17]([OH:19])=[O:18])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 18542632HCID 18542632, 화합물

생성물 1

HCID 18542720HCID 18542720, 화합물수율 40.9%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
40 °C

실험 절차

A solution of dimethyl 2-(1-t-butoxycarbonylpiperidin-4-yloxy)-5-nitroisophthalate (10.7 g) in concentrated hydrochloric acid (100 ml) was stirred at 80° C. for 10 hours. The reaction mixture was concentrated in vacuo. To the residue was added hexane to afford a white solid which was collected by filtration. To a solution of the solid in a mixture of water (50 ml) and acetone (50 ml) were added sodium hydrogencarbonate (4.6 g) and di-t-butyl dicarbonate (5.9 g) at room temperature. The resulting mixture was stirred at 40° C. for 1 hour. The reaction mixture was extracted with ethyl acetate. The extract was washed with brine. The organic layer was dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated in vacuo. To the residue was added hexane and the mixture was filtered to give the desired compound (4.1 g, yield 40%) as a pale yellow solid.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionTo the residue was added hexane
  3. customto afford a white solid which
  4. filtrationwas collected by filtration
  5. additionTo a solution of the solid in a mixture of water (50 ml) and acetone (50 ml)
  6. additionwere added sodium hydrogencarbonate (4.6 g) and di-t-butyl dicarbonate (5.9 g) at room temperature
  7. extractionThe reaction mixture was extracted with ethyl acetate
  8. washThe extract was washed with brine
  9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. concentrationthe filtrate was concentrated in vacuo
  12. additionTo the residue was added hexane
  13. filtrationthe mixture was filtered

출처 및 근거

ORD 기록
ord-7227a9e683c1404aac6c9c450ebf98ab
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06555556B1

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