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

HRID 376293ノート

反応式

HRID 376293 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4086eb7de1be46608c105d917d10e42e
出典データセット
uspto-grants-2000_02
特許番号
US06020345

反応ノート

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