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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 66732297, 화합물

HRID 1963166
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반응식

HRID 1963166 반응식
[C:1]([C:5]1[S:9][C:8]([C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][N:19]=2)[C:13]([O:15][CH3:16])=[O:14])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[ClH:20]>[Pt](=O)=O>[ClH:20].[C:1]([C:5]1[S:9][C:8]([CH:10]2[CH2:11][CH:12]([C:13]([O:15][CH3:16])=[O:14])[CH2:17][CH2:18][NH:19]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66732183HCID 66732183, 화합물

생성물 1

HCID 66732297HCID 66732297, 화합물수율 101.1%

시약·촉매·용매 1

HCID 345198Adams' catalyst촉매4회

실험 절차

Methyl 2-(5-tert-butylthiophen-2-yl)isonicotinate (2.02 g, 7.34 mmol) was dissolved in hydrogen chloride (1.25 M in MeOH, 11.74 mL, 14.67 mmol) and stirred at room temperature for 30 min. The solvent was evaporated in vacuo. The residue was dissolved in MeOH (20 mL), platinum(IV) oxide (0.050 g, 0.22 mmol) added and the reaction mixture hydrogenated in a Büchi hydrogenator at 5 bar and room temperature for 3 h. Additional platinum(IV) oxide (0.050 g, 0.22 mmol) was added and the hydrogenation continued for 3 h. The reaction mixture was filtered through celite, washed with MeOH and the filtrate evaporated in vacuo. The residue was redissolved in MeOH (15 mL) and platinum(IV) oxide (0.167 g, 0.73 mmol) added. Hydrogenation was continued for 3 h. Additional platinum(IV) oxide (0.167 g, 0.73 mmol) was added and the hydrogenation continued for 2 h. The reaction mixture was filtered through celite, washed with MeOH and the filtrate evaporated in vacuo to yield methyl 2-(5-tert-butylthiophen-2-yl)piperidine-4-carboxylate hydrochloride (2.360 g, 101%) as a black oil. MS m/z 282 (M+H)+

후처리

  1. customThe solvent was evaporated in vacuo
  2. dissolutionThe residue was dissolved in MeOH (20 mL)
  3. waitthe reaction mixture hydrogenated in a Büchi hydrogenator at 5 bar and room temperature for 3 h
  4. waitthe hydrogenation continued for 3 h
  5. filtrationThe reaction mixture was filtered through celite
  6. washwashed with MeOH
  7. customthe filtrate evaporated in vacuo
  8. dissolutionThe residue was redissolved in MeOH (15 mL)
  9. waitHydrogenation was continued for 3 h
  10. waitthe hydrogenation continued for 2 h
  11. filtrationThe reaction mixture was filtered through celite
  12. washwashed with MeOH
  13. customthe filtrate evaporated in vacuo

출처 및 근거

ORD 기록
ord-0b1575e58c3b481b86a12d9378c21c86
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415378B2

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