4-Methylmorpholine → (Z)-tert-butyl 3-(4-(2-methoxyethyl)phenoxy)acrylate

HRID 919020

反応式

HRID 919020 の反応式
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.[C:12]([O:16][C:17](=[O:20])[C:18]#[CH:19])([CH3:15])([CH3:14])[CH3:13].CN1CCOCC1>C(Cl)Cl>[CH3:1][O:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11]/[CH:19]=[CH:18]\[C:17]([O:16][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:20])=[CH:7][CH:6]=1

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 925164-(2-Methoxyethyl)phenolHCID 543038tert-Butyl propiolate

生成物 1

HCID 67168776(Z)-tert-butyl 3-(4-(2-methoxyethyl)phenoxy)acrylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

a mixture of 4-(2-methoxy ethyl)phenol (1.547 g, 10.3 mmol), propiolic acid tert-butyl ester (1.367 g, 10.8 mmol) and N-methyl morpholine (1.18 mL, 10.8 mmol) in CH2Cl2 (15 mL) was stirred at room temperature for 24 hours. The mixture was absorbed on SiO2 (20 g) and purified by column chromatography using a mixture of methylene chloride/hexane. The product was obtained as a two to one mixture of (E)/(Z)-tert-butyl 3-(4-(2-methoxyethyl)phenoxy)acrylate isomers (2.0 g).

後処理

  1. customThe mixture was absorbed on SiO2 (20 g)
  2. custompurified by column chromatography
  3. additiona mixture of methylene chloride/hexane

出典と根拠

ORDレコード
ord-27fe801f7c40487d879d71328d0bfc47
出典データセット
uspto-grants-2016_03
特許番号
US09272996B2

関連ノート

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