Potassium Carbonate → 2-[1,3]Dioxolan-2-yl-6-oxazol-5-yl-pyridine

HRID 376293노트

반응식

HRID 376293 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[N:11]=[C:10]([CH:12]=[O:13])[CH:9]=[CH:8][CH:7]=1.S([CH2:24][N:25]=[C:26]=O)(C1C=CC(C)=CC=1)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>CO>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:7]=[CH:8][CH:9]=[C:10]([C:12]2[O:13][CH:26]=[N:25][CH:24]=2)[N:11]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 117890781-Isocyanatomethanesulfonyl-4-methylbenzeneHCID 193617196-[1,3]Dioxolan-2-yl-pyridine-2-carbaldehyde

생성물 1

HCID 105607472-[1,3]Dioxolan-2-yl-6-oxazol-5-yl-pyridine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1 g of 6-[1,3]dioxolan-2-yl-pyridine-2-carbaldehyde (5.58 mmol), 1.10 g of tosylmethyl isocyanate (5.63 mmol) and 0.80 g of potassium carbonate (5.79 mmol) are mixed in 15 ml of methanol. The suspension is heated under reflux for 2 hours. The methanol is separated off, the residue is taken up in a saturated aqueous solution of sodium chloride and the mixture is extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered and then concentrated under vacuum. The title product is isolated by chromatography on a silica column (eluent: hexane/ethyl acetate; 50:50). 1.14 g of a yellow oil are obtained.

후처리

  1. temperatureThe suspension is heated
  2. temperatureunder reflux for 2 hours
  3. customThe methanol is separated off
  4. extractionthe mixture is extracted with ethyl acetate
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-4086eb7de1be46608c105d917d10e42e
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06020345

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