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Epichlorohydrin → HCID 21450254, 화합물

HRID 596681
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HRID 596681 반응식
[CH2:1]([C:4]1[CH:5]=[C:6]([C:11]2[CH2:12][CH2:13][C:14](=[O:17])[NH:15][N:16]=2)[CH:7]=[CH:8][C:9]=1[OH:10])[CH:2]=[CH2:3].[CH2:18]([CH:20]1[O:22][CH2:21]1)Cl.OC1C=CC=CC=1C(CCC(O)=O)=O.[OH-].[Na+]>ClCCl>[CH2:1]([C:4]1[CH:5]=[C:6]([C:11]2[CH2:12][CH2:13][C:14](=[O:17])[NH:15][N:16]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH2:18][CH:20]1[O:22][CH2:21]1)[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7835EpichlorohydrinHCID 14798Sodium HydroxideHCID 30160863-(2-Hydroxybenzoyl)propionic acidHCID 1355732836-(3-allyl-4-hydroxyphenyl)-4,5-dihydro-3(2H)-pyridazinone

생성물 1

HCID 21450254HCID 21450254, 화합물수율 47%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

A mixture of finely ground 6-(3-allyl-4-hydroxyphenyl)-4,5-dihydro-3(2H)-pyridazinone (50g, 0.22 mole), epichlorohydrin (200 g, 2.2 mole) and piperidine (2g) was heated on a steam bath for 90 minutes. Evaporation under reduced pressure gave a viscous oil which was dissolved in dichloromethane and stirred for 10 minutes with dilute sodium hydroxide (500 ml). The organic phase was washed with water, dried and evaporated to an oil which slowly solidified. Addition of ethanol-ether gave 6[3-allyl-4-(2,3-epoxypropoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone (30g, 47%, m.p. 92.5°-95° C) which was recrystallised from aqueous ethanol to give the pure pyridazinone (m.p. 93.5°-95° C).

후처리

  1. temperaturewas heated on a steam bath for 90 minutes
  2. customEvaporation under reduced pressure
  3. customgave a viscous oil which
  4. washThe organic phase was washed with water
  5. customdried
  6. customevaporated to an oil which
  7. additionAddition of ethanol-ether

출처 및 근거

ORD 기록
ord-a2da714099554429bb63ad349a11e8a3
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04011321

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