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

HRID 723280노트

반응식

HRID 723280 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 10942334Sodium Methoxide촉매HCID 1140Toluene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-39cdc5cb1477411e99c388126cee1a67
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141351B2

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