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Ethanol → HCID 20031327, 화합물

HRID 232286
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HRID 232286 반응식
[CH2:1]([OH:3])[CH3:2].[CH2:4]([CH:6]1[O:8][CH2:7]1)Cl.[CH2:9]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[OH-].[Na+]>CCOCC.[Cl-].[Zn+2].[Cl-].O>[CH2:1]([O:3][CH2:4][CH:6]([OH:8])[CH2:7][N:18]1[CH2:19][CH2:20][N:15]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:16][CH2:17]1)[CH3:2]
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참가 물질

8

반응물 4

HCID 702EthanolHCID 7835EpichlorohydrinHCID 14798Sodium HydroxideHCID 27365131-Hexylpiperazine

생성물 1

HCID 20031327HCID 20031327, 화합물

시약·촉매·용매 3

HCID 3007855Zincchloride촉매HCID 962
Water
용매
HCID 3283Diethyl Ether용매

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온도
100 °C

실험 절차

To 100 mL of ethanol add 87 g (0.1 mol) of epichlorohydrin and zinc chloride (1 mL of a 0.872M solution in ether). Stir the reaction mixture at 100° C. for 2 days at which time remove the heat source and add 17.0 g (0.1 mol) of 1-hexyl-piperazine and 20 mL of 50% aqueous sodium hydroxide. Heat the reaction for 3 hours. Add 100 mL of water and extract twice with 200 mL of ether. Combine the organic layers and dry over Na2SO4. Remove the drying agent by filtration and evaporate the solvent in vacuo to obtain the title compound.

후처리

  1. customremove the heat source
  2. temperatureHeat
  3. customthe reaction for 3 hours
  4. extractionextract twice with 200 mL of ether
  5. dry with materialdry over Na2SO4
  6. customRemove the drying agent
  7. filtrationby filtration
  8. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-0b7b9ae01a2941eebf77d020829cd480
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851526

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