Potassium Carbonate → 1-(2-Hydroxypropyl)-1H-pyrazole-4-carboxaldehyde

HRID 220486노트

반응식

HRID 220486 반응식
[NH:1]1[CH:5]=[C:4]([CH:6]=[O:7])[CH:3]=[N:2]1.Br[CH2:9][CH:10]([OH:12])[CH3:11].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[OH:12][CH:10]([CH3:11])[CH2:9][N:1]1[CH:5]=[C:4]([CH:6]=[O:7])[CH:3]=[N:2]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 297401-Bromo-2-propanolHCID 51306731H-pyrazole-4-carbaldehyde

생성물 1

HCID 875099441-(2-Hydroxypropyl)-1H-pyrazole-4-carboxaldehyde

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
150 °C

실험 절차

Combine 1H-pyrazole-4-carbaldehyde (0.150 g, 1.56 mmol), racemic 1-bromo-2-propanol (0.260 g, 1.87 mmol), and potassium carbonate (0.323 g, 2.34 mmol) in acetonitrile (2 mL). Heat in microwave at 150° C. for 20 min. Filter, wash with acetonitrile and concentrate filtrate. Purify via silica gel chromatography, eluting with 0:100 to 100:0 ethyl acetate:hexanes) to give the title preparation (177 mg, 73%). GC-MS: m/z=154 [M+].

후처리

  1. filtrationFilter
  2. washwash with acetonitrile
  3. concentrationconcentrate filtrate
  4. customPurify via silica gel chromatography
  5. washeluting with 0:100 to 100:0 ethyl acetate
  6. customhexanes) to give the title
  7. custompreparation (177 mg, 73%)

출처 및 근거

ORD 기록
ord-ed4bf177d43f4255acb295070f6f56a9
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202873B2

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