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1-Phenethylamine → HCID 19019336、化合物

HRID 2081670
ノート
印刷プレビュー

反応式

HRID 2081670 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 74081-PhenethylamineHCID 10340Sodium CarbonateHCID 253877Potassium BromideHCID 14749912HCID 14749912、化合物

生成物 1

HCID 19019336HCID 19019336、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-0c928793d40748728008281ed544a38e
出典データセット
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05185352

反応ノート

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