Epichlorohydrin → 1,2-Epoxy-3-[3-(2-pyridylmethyl)phenoxy]propane

HRID 1075855노트

반응식

HRID 1075855 반응식
[CH2:1]([CH:3]1[O:5][CH2:4]1)Cl.[N:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]1[CH:14]=[C:15]([OH:19])[CH:16]=[CH:17][CH:18]=1.[OH-].[Na+]>CO>[O:5]1[CH:3]([CH2:1][O:19][C:15]2[CH:16]=[CH:17][CH:18]=[C:13]([CH2:12][C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][N:6]=3)[CH:14]=2)[CH2:4]1

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 14798Sodium HydroxideHCID 215413183-[(Pyridin-2-yl)methyl]phenol

생성물 1

HCID 129198521,2-Epoxy-3-[3-(2-pyridylmethyl)phenoxy]propane수율 62.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

19 g of epichlorohydrin is added to a mixture of 18.5 g of 3-(2-pyridylmethyl)phenol, 4.2 g of sodium hydroxide and 200 ml of methanol, and the resulting mixture is stirred at about 50°C for 3 hours. The methanol is then removed, water is added to the residue, and the aqueous solution is extracted with 200 ml of benzene. The benzene layer is washed with 5% sodium hydroxide and with water, and dried over anhydrous magnesium sulfate. The benzene is removed to give 15.0 g of 1,2-epoxy-3-[3-(2-pyridylmethyl)-phenoxy] propane as oil.

후처리

  1. customThe methanol is then removed
  2. additionwater is added to the residue
  3. extractionthe aqueous solution is extracted with 200 ml of benzene
  4. washThe benzene layer is washed with 5% sodium hydroxide and with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe benzene is removed

출처 및 근거

ORD 기록
ord-96f42c65db9e4ce5a0987d605fb71031
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03954776

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