4-Hydroxybenzaldehyde → HCID 10242087, 화합물

HRID 629132

반응식

HRID 629132 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.Cl[CH2:11][CH2:12][C:13]([CH3:16])([CH3:15])[CH3:14].[I-].[Na+].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[CH3:14][C:13]([CH3:16])([CH3:15])[CH2:12][CH2:11][O:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 761111-Chloro-3,3-dimethylbutane

생성물 1

HCID 10242087HCID 10242087, 화합물수율 78%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A suspension of 4-hydroxybenzaldehyde (200 mg, 1.64 mmol), 1-chloro-3,3-dimethylbutane (395 mg, 1.97 mmol), sodium iodide (24 mg, 0.16 mmol), and cesium carbonate (800 mg, 2.46 mmol) in anhydrous dimethylformamide (5 mL) was stirred at 80° C. overnight. After cooling to room temperature, solids were filtered and washed with ether. The filtrate was washed with 2 N sodium hydroxide (2×20 mL), water (20 mL), and brine (20 mL), dried over magnesium sulfate, filtered, and concentrated to give 4-(3,3-dimethylbutoxyl)benzaldehyde (262 mg, 78% crude) as a pale yellow oil that was used without further purification or characterization.

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationsolids were filtered
  3. washwashed with ether
  4. washThe filtrate was washed with 2 N sodium hydroxide (2×20 mL), water (20 mL), and brine (20 mL)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-23997737ec954abd986e8cd86c56a09a
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315495B2

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