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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 66778542, 화합물 → HCID 56847101, 화합물

HRID 1261730
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HRID 1261730 반응식
[ClH:1].C([N:9]1[CH2:18][CH2:17][C:16]2[N:15]=[C:14]([C:19]([O:21][CH3:22])=[O:20])[CH:13]=[CH:12][C:11]=2[CH2:10]1)C1C=CC=CC=1>CO.[OH-].[Pd+2].[OH-]>[ClH:1].[N:15]1[C:16]2[CH2:17][CH2:18][NH:9][CH2:10][C:11]=2[CH:12]=[CH:13][C:14]=1[C:19]([O:21][CH3:22])=[O:20]
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참가 물질

4

반응물 1

HCID 66778542HCID 66778542, 화합물

생성물 1

HCID 56847101HCID 56847101, 화합물수율 112.8%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매

실험 절차

The crude methyl 6-benzyl-5,6,7,8-tetrahydro-1,6-naphthyridine-2-carboxylate hydrochloride (1.20 g, 3.76 mmol) was dissolved in MeOH (100 mL) and thoroughly degassed. Palladium hydroxide (0.185 g, 1.32 mmol) was added to the solution before being purged with H2 gas three times. The reaction was allowed to stir at rt for 13 h under 1 atm of H2 gas. The mixture was then filtered through a pad of Celite and rinsed with EtOH. The filtrate was then concentrated down to yield methyl 5,6,7,8-tetrahydro-1,6-naphthyridine-2-carboxylate hydrochloride (0.97 g, 100%). LC-MS: (FA) ES+ 220; 1H NMR (Methanol-d4, 400 MHz) δ 8.05 (d, J=8.0 Hz, 1H), 7.89 (d, J=8.0 Hz, 1H), 4.52 (s, 2H), 3.98 (s, 3H), 3.66 (t, J=6.5 Hz, 2H), 3.33 (m, 2H).

후처리

  1. customthoroughly degassed
  2. custombefore being purged with H2 gas three times
  3. filtrationThe mixture was then filtered through a pad of Celite
  4. washrinsed with EtOH
  5. concentrationThe filtrate was then concentrated down

출처 및 근거

ORD 기록
ord-a96da926eae24a41962a8699e385dd64
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08471026B2

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