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Methanol → HCID 14989569, 화합물

HRID 2248462
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HRID 2248462 반응식
[CH3:1][O-:2].[Na+].Cl.[NH2:5][C:6]1([C:12]2[CH:13]=[CH:14][C:15](=[O:18])[NH:16][CH:17]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[CH3:19]O>>[O:18]=[C:15]1[NH:16][CH:17]=[C:12]([C:6]2([NH:5][C:1](=[O:2])[CH3:19])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[CH:13]=[CH:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 19768457HCID 19768457, 화합물

생성물 1

HCID 14989569HCID 14989569, 화합물

실험 절차

Sodium methoxide solution (25% in methanol, 6 ml) was added to a suspension of 5-(1-aminocyclohexyl)-2(1H)-pyridinone hydrochloride (6.0 g) in 100 ml of methanol, and the mixture was stirred at room temperature for 10 minutes. The solvent was removed in vacuo, and the residual solids were suspended in 260 ml of dichloromethane. Poly-4-vinylpyridine (5.42 g), acetic anhydride (2.67 g) and a catalytic amount of 4-(N,N-dimethylamino)pyridine were added, and the mixture was stirred at room temperature for 2 hours. The suspension was filtered and the solid residue was washed with methanol. The filtrate was concentrated, leaving 4.9 g of solid. Recrystallization from methanol gave 1.69 g of product (m.p. 238°-242° C. dec) in two crops, each of which was analytically pure.

후처리

  1. customThe solvent was removed in vacuo
  2. additionPoly-4-vinylpyridine (5.42 g), acetic anhydride (2.67 g) and a catalytic amount of 4-(N,N-dimethylamino)pyridine were added
  3. stirringthe mixture was stirred at room temperature for 2 hours
  4. filtrationThe suspension was filtered
  5. washthe solid residue was washed with methanol
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-64ef7de655f34fffa288b2004e9cc729
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05039809

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