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1-Phenethylamine → HCID 19019336, 화합물

HRID 2081670
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HRID 2081670 반응식
[OH:1][CH2:2][C:3]1O[CH:5]=[C:6]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7](=[O:9])[CH:8]=1.[C:29]1([CH:35]([NH2:37])[CH3:36])[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C([O-])([O-])=O.[Na+].[Na+].[K+].[Br-]>C(O)C.O>[OH:1][CH2:2][C:3]1[N:37]([CH:35]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH3:36])[CH:5]=[C:6]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7](=[O:9])[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 74081-PhenethylamineHCID 10340Sodium CarbonateHCID 253877Potassium BromideHCID 14749912HCID 14749912, 화합물

생성물 1

HCID 19019336HCID 19019336, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 962
Water
용매

실험 절차

A mixture of 8.0 g (0.02 Mol) 2-hydroxymethyl-5-octadecyloxy-4-pyranone, 4.8 g (0.04 Mol) (±)-1-phenylethylamine, 1.5 g Na2CO3, 10 mL water and 100 mL ethanol is boiled under reflux for 72 hours. After cooling the solvent and the excess of amine is removed under vacuum and the residue is mixed with water and extracted with dichloromethane. The organic phase is dried over Na2SO4, evaporated and the obtained resin is purified by column chromatography on silica gel with dichloromethane with 1-2% methanol to give a yellow oil, which is changing to wax-like consistency. IR (KBr): 1630 (C=O), MS (m/l) 497 (M+).

후처리

  1. temperatureunder reflux for 72 hours
  2. temperatureAfter cooling the solvent
  3. customthe excess of amine is removed under vacuum
  4. additionthe residue is mixed with water
  5. extractionextracted with dichloromethane
  6. dry with materialThe organic phase is dried over Na2SO4
  7. customevaporated
  8. customthe obtained resin is purified by column chromatography on silica gel with dichloromethane with 1-2% methanol
  9. customto give a yellow oil, which

출처 및 근거

ORD 기록
ord-0c928793d40748728008281ed544a38e
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05185352

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