N-(2-Hydroxyethyl)imidazole → 2-(1H-Imidazol-1-yl)ethyl methoxyacetate

HRID 723280ノート

反応式

HRID 723280 の反応式
[N:1]1([CH2:6][CH2:7][OH:8])[CH:5]=[CH:4][N:3]=[CH:2]1.[CH3:9][O:10][CH2:11][C:12](OC)=[O:13]>C[O-].[Na+].C1(C)C=CC=CC=1>[CH3:9][O:10][CH2:11][C:12]([O:8][CH2:7][CH2:6][N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)=[O:13]

参加物

5

反応物 2

HCID 74168N-(2-Hydroxyethyl)imidazoleHCID 80507Methyl methoxyacetate

生成物 1

HCID 218725332-(1H-Imidazol-1-yl)ethyl methoxyacetate収率 90.2%

試薬・触媒・溶媒 2

HCID 10942334Sodium Methoxide触媒HCID 1140Toluene溶媒

実験手順

In a nitrogen atmosphere, a mixture of 112 g of 2-(1H-imidazol-1-yl)ethanol, synthesized in Synthesis Example 1, 156 g of methyl methoxyacetate, 3.0 g of sodium methoxide, and 200 g of toluene was heated under reflux for 20 hours while distilling off the methanol formed during the reaction. The solvent was distilled off in vacuo. Purification by vacuum distillation gave 166 g of 2-(1H-imidazol-1-yl)ethyl methoxyacetate (boiling point 126° C./27 Pa, yield 90%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hours
  3. distillationwhile distilling off the methanol
  4. customformed during the reaction
  5. distillationThe solvent was distilled off in vacuo
  6. customPurification
  7. distillationby vacuum distillation

出典と根拠

ORDレコード
ord-39cdc5cb1477411e99c388126cee1a67
出典データセット
uspto-grants-2006_11
特許番号
US07141351B2

反応ノート

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