Dimethylformamide → HCID 18473977, 화합물

HRID 2227526노트

반응식

HRID 2227526 반응식
[CH3:1][N:2]([CH3:21])[C:3]1[O:4][CH:5]([CH:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[OH:20])[NH:13][CH:12]=2)[CH3:10])[C:6](=[O:8])[N:7]=1.[CH3:22]N(C)C=O.C(=O)([O-])[O-].[K+].[K+]>O>[CH3:21][N:2]([CH3:1])[C:3]1[O:4][CH:5]([CH:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[O:20][CH3:22])[NH:13][CH:12]=2)[CH3:10])[C:6](=[O:8])[N:7]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 184739322-(Dimethylamino)-5-[1-(4-hydroxy-1H-indol-3-yl)ethyl]-4(5H)-oxazolone

생성물 1

HCID 18473977HCID 18473977, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-dimethylamino-5-[1-(4-hydroxyindol-3-yl)ethyl]2-oxazolin-4-one (120 mg) was dissolved into dimethylformamide (3 ml). Potassium carbonate (115 mg) and indomethane (156 l) were added. The mixture was stirred for 3 hours at room temperature and additional indomethane (78 μl) was added. The mixture was stirred for 36 hours at room temperature. To the reaction mixture was added water and the whole was extracted with ethyl acetate. The extract was washed with brine and dried over magnesium sulfate. Concentration of the ethyl acetate solution gave a residue, which was subjected to silica gel chromatography. Elution with hexane-acetone (1:1) provided 2-dimethylamino-5-[1-(4-methoxyindol-3-yl)ethyl]-2-oxazolin-4-one (54 mg).

후처리

  1. additionadditional indomethane (78 μl) was added
  2. stirringThe mixture was stirred for 36 hours at room temperature
  3. extractionthe whole was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customConcentration of the ethyl acetate solution gave a residue, which
  7. washElution with hexane-acetone (1:1)

출처 및 근거

ORD 기록
ord-b9ed3d3e990f4a74a154a8ba0401746e
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06414003B1

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