Sodium Azide → Methyl 2-azido-2-methoxyacetate

HRID 1658003노트

반응식

HRID 1658003 반응식
Cl[CH:2]([O:7][CH3:8])[C:3]([O:5][CH3:6])=[O:4].[N-:9]=[N+:10]=[N-:11].[Na+]>C(COC)OC>[N:9]([CH:2]([O:7][CH3:8])[C:3]([O:5][CH3:6])=[O:4])=[N+:10]=[N-:11]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 11018941Methyl 2-chloro-2-methoxy-acetate

생성물 1

HCID 20357785Methyl 2-azido-2-methoxyacetate수율 72.4%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of methyl 2-chloro-2-methoxyacetate (13.86 g., 0.1 mole), powdered sodium azide (8.46 g., 0.13 mole) and dry dimethoxyethane (80ml.) is stirred and heated at reflux for 39 hours. After cooling to room temperature, the mixture is filtered to remove salts which are washed with dry ether. Evaporation of the solvents at aspirator pressure leaves a yellow liquid which is distilled to give methyl 2-azido-2-methoxyacetate (10.5 g.) as a water-white liquid (b.p. 75°-77°C./17 mm.).

후처리

  1. temperatureheated
  2. temperatureat reflux for 39 hours
  3. filtrationthe mixture is filtered
  4. customto remove salts which
  5. washare washed with dry ether
  6. customEvaporation of the solvents at aspirator pressure
  7. customleaves a yellow liquid which
  8. distillationis distilled

출처 및 근거

ORD 기록
ord-4eede6886068485f9df11ad30c1b9b70
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03962224

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