Phosphoric Acid → 3-(6-Bromopyridin-2-yl)-2,3-dimethylbutan-2-ol

HRID 1630387노트

반응식

HRID 1630387 반응식
C[Mg]I.C([O:6][CH2:7][CH3:8])C.[CH2:9](OCC)C.[Br:14][C:15]1[N:20]=[C:19]([C:21](C)([CH3:27])[C:22](OCC)=O)[CH:18]=[CH:17][CH:16]=1.P(=O)(O)(O)O>O>[Br:14][C:15]1[N:20]=[C:19]([C:21]([CH3:22])([CH3:27])[C:7]([CH3:8])([OH:6])[CH3:9])[CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 1004Phosphoric AcidHCID 3283Diethyl EtherHCID 86616118Ethyl 2-(6-bromopyridin-2-yl)-2-methylpropionateHCID 178467823HCID 178467823, 화합물

생성물 1

HCID 866161193-(6-Bromopyridin-2-yl)-2,3-dimethylbutan-2-ol

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In a nitrogen atmosphere, 13 mL of 2 M methylmagnesium iodide/diethyl ether solution was added to diethyl ether (20 mL) solution of 2.72 g of ethyl 2-(6-bromopyridin-2-yl)-2-methylpropionate with cooling in an ice bath. The reaction liquid was stirred at room temperature for 3 hours, and then water and aqueous 10% phosphoric acid solution were added thereto, extracted with diethyl ether, washed with aqueous saturated sodium hydrogencarbonate solution and saturated saline water, and then dried with anhydrous magnesium sulfate. After concentrated under reduced pressure, the residue was purified through silica gel column chromatography (hexane/ethyl acetate=9/1 to 8/1) to obtain 1.47 g of the entitled compound as a colorless oily substance.

후처리

  1. temperaturewith cooling in an ice bath
  2. customThe reaction liquid
  3. extractionextracted with diethyl ether
  4. washwashed with aqueous saturated sodium hydrogencarbonate solution and saturated saline water
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationAfter concentrated under reduced pressure
  7. customthe residue was purified through silica gel column chromatography (hexane/ethyl acetate=9/1 to 8/1)

출처 및 근거

ORD 기록
ord-4aaf1a64372a4aac90e9e92f08995df0
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791125B2

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