Dimethylformamide → HCID 19068171, 화합물

HRID 1957576노트

반응식

HRID 1957576 반응식
[OH:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[O:4][N:3]=1.[C:11]([N:18]1[CH2:23][CH2:22][CH:21]([CH2:24][CH2:25][CH2:26]I)[CH2:20][CH2:19]1)([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12].C([O-])([O-])=O.[Cs+].[Cs+].CN(C=O)C>CCOCC>[C:11]([N:18]1[CH2:19][CH2:20][CH:21]([CH2:24][CH2:25][CH2:26][O:1][C:2]2[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[O:4][N:3]=2)[CH2:22][CH2:23]1)([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 9975355Tert-butyl 4-(3-iodopropyl)piperidine-1-carboxylateHCID 178498603HCID 178498603, 화합물

생성물 1

HCID 19068171HCID 19068171, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of methyl 3-hydroxy-5-isoxazolecarboxylate (Aldrich) (3-5) (286 mg, 2.0 mmol), 3-4 (706 mg, 2.0 mmol), Cs2CO3 (650 mg, 2.0 mmol), and DMF (10 mL) was stirred at ambient temperature. After 72 hours the reaction mixture was diluted with ether and then washed with H2O and brine, dried (MgSO4), and concentrated. Flash chromatography (silica, 4% acetone/CH2Cl2) gave 3-6 as a colorless solid. Rf 0.54 (silica, 40 %EtOAc/hexanes).

후처리

  1. washwashed with H2O and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-18110f652a764c16bd5b52672752c62f
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786373

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