Epichlorohydrin → 1-Benzyloxy-4-(2,3-epoxypropyl)-naphthyl ether

HRID 2247846

반응식

HRID 2247846 반응식
O[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:4][CH:3]=1.[CH2:20]([CH:22]1[O:24][CH2:23]1)Cl.[OH-:25].[Na+]>O>[CH2:13]([O:12][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([CH2:20][CH:22]2[O:24][CH2:23]2)=[CH:3][C:4]=1[O:25][C:4]1[CH:3]=[C:2]([CH2:20][CH:22]2[O:24][CH2:23]2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]=1[O:12][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 14798Sodium HydroxideHCID 5629374-(Benzyloxy)naphthalen-1-ol

생성물 1

HCID 572662001-Benzyloxy-4-(2,3-epoxypropyl)-naphthyl ether

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of 4.3 g. (0.017 mole) 1-hydroxy-4-benzyloxynaphthalene in 15 ml. (0.19 mole) epichlorohydrin, which is heated to its boiling point while stirring, is carefully added dropwise 3.7 ml. 5M aqueous sodium hydroxide solution (0.0187 mole). The apparatus used for carrying out the reaction is equipped with a water separator so that the water distils off azeotropically from the reaction mixture with epichlorohydrin. After distilling off the theoretical amount of water, the reaction mixture is further heated under reflux for 1 hour while stirring, thereafter mixed with 50 ml. toluene, filtered off from inorganic components and the solution evaporated on a rotary evaporator. The product obtained is used for the next reaction step without further purification. Yield 6.1 g.

후처리

  1. additionis carefully added dropwise 3.7 ml
  2. customdistils off azeotropically from the reaction mixture with epichlorohydrin
  3. distillationAfter distilling off the theoretical amount of water
  4. temperaturethe reaction mixture is further heated
  5. temperatureunder reflux for 1 hour
  6. stirringwhile stirring
  7. additionmixed with 50 ml
  8. filtrationtoluene, filtered off from inorganic components
  9. customthe solution evaporated on a rotary evaporator
  10. customThe product obtained
  11. customis used for the next reaction step without further purification

출처 및 근거

ORD 기록
ord-a7db72b6b20d4e5e8c4103c466e52550
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037828

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