Phenol → HCID 13055710, 화합물

HRID 2198846노트

반응식

HRID 2198846 반응식
[CH:1]([N:4]1[CH2:7][CH:6]([O:8][CH2:9][O:10][CH3:11])[CH2:5]1)([CH3:3])[CH3:2].[C:12]1([OH:18])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[OH-].[Na+]>CCOCC>[O:18]([CH2:5][CH:6]([O:8][CH2:9][O:10][CH3:11])[CH2:7][NH:4][CH:1]([CH3:2])[CH3:3])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 996PhenolHCID 14798Sodium HydroxideHCID 205173143-(Methoxymethoxy)-1-(propan-2-yl)azetidine

생성물 1

HCID 13055710HCID 13055710, 화합물수율 67%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
180 °C

실험 절차

To a mixture of 1.6 parts of 1-iso-propyl-3-methoxymethoxyazetidine and 9.4 parts of phenol 0.5 part of sodium hydroxide was addded, and the mixture was heated at 180° C. for 6 hours. The reaction mixture was cooled and 100 parts of ether were added thereto. Excessive phenol was removed by extraction with 2 N-sodium hydroxide aqueous solution, and the remaining ether layer was washed in water and dried over anhydrous sodium sulfate. After distillation of ether, the residue was subjected to distillation to yield 1.6 parts of 1-phenoxy-2-methoxymethoxy-3-(iso-propylamino)-propane boiling at 146°-149° C. under 2 mm Hg. The yield was 67%.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customExcessive phenol was removed by extraction with 2 N-sodium hydroxide aqueous solution
  3. washthe remaining ether layer was washed in water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationAfter distillation of ether
  6. distillationthe residue was subjected to distillation

출처 및 근거

ORD 기록
ord-2c1f4e08a2ae4f29958bfbdb7772391f
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04360464

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