Potassium Carbonate → HCID 22281971, 화합물

HRID 1368661노트

반응식

HRID 1368661 반응식
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([OH:8])[C:3]=1[C:9]1[CH:17]=[CH:16][C:12]2[O:13][CH2:14][O:15][C:11]=2[CH:10]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][CH:26]1[CH2:28][CH2:27]1>CN(C)C=O>[O:13]1[C:12]2[CH:16]=[CH:17][C:9]([C:3]3[C:4]([O:8][CH2:25][CH:26]4[CH2:28][CH2:27]4)=[N:5][N:6]([CH3:7])[C:2]=3[NH2:1])=[CH:10][C:11]=2[O:15][CH2:14]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 178481945HCID 178481945, 화합물

생성물 1

HCID 22281971HCID 22281971, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 5-amino-4-(1,3-benzodioxol-5-yl)-1-methyl-1H-pyrazol-3-ol (500 mg) (Preparation 46) in anhydrous dimethylformamide (21 ml) under an atmosphere of nitrogen at room temperature was added solid potassium carbonate (980 mg) and bromomethylcyclopropane (230 μl). The mixture was stirred overnight then quenched by the addition of water (100 ml) and a saturated aqueous solution of ammonium chloride (50 ml). The solution was extracted with ethyl acetate (3×40 ml). The organic fraction was dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica, 30 g) eluted with hexane:ethyl acetate (1:2) to yield the title compound as a colourless oil (365 mg).

후처리

  1. customthen quenched by the addition of water (100 ml)
  2. extractionThe solution was extracted with ethyl acetate (3×40 ml)
  3. dry with materialThe organic fraction was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography (silica, 30 g)
  6. washeluted with hexane:ethyl acetate (1:2)

출처 및 근거

ORD 기록
ord-fb4c9adf15fd43cfa5c4338849e1a701
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06573270B1

반응 노트

불러오는 중…