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Pyridine → HCID 18969790, 화합물

HRID 399075
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HRID 399075 반응식
[CH3:1][C:2]1([CH3:23])[CH:5]([OH:6])[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[C:3]1[C:13]1[CH:18]=[CH:17][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1.N1C=CC=CC=1.[CH3:30][C:31](OC(C)=O)=[O:32]>C(Cl)Cl.CN(C1C=CN=CC=1)C.CCOC(C)=O.O>[CH3:1][C:2]1([CH3:23])[CH:5]([O:6][C:31](=[O:32])[CH3:30])[C:4]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[C:3]1[C:13]1[CH:14]=[CH:15][C:16]([S:19]([CH3:22])(=[O:21])=[O:20])=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 18969768HCID 18969768, 화합물

생성물 1

HCID 18969790HCID 18969790, 화합물

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매
HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of Example 62 (150 mg) in CH2Cl2 (3 mL) at r.t., was added pyridine (370 mL), Ac2O (215 μL) and DMAP (5 mg). The mixture was stirred at r.t. for 2 hr and diluted with EtOAc and H2O. The organic phase was washed with HCl 1N, brine, dried (MgSO4) and the solvents evaporated. The residue was purified by flash chromatography (silica gel; hexane/EtOAc (70:30)) to give the title compound as a white solid, m.p. 60°-61° C.

후처리

  1. washThe organic phase was washed with HCl 1N, brine
  2. dry with materialdried (MgSO4)
  3. customthe solvents evaporated
  4. customThe residue was purified by flash chromatography (silica gel; hexane/EtOAc (70:30))

출처 및 근거

ORD 기록
ord-41a3ca67a7ba40559bb09c013b5fd1dc
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05817700

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