Sodium Azide → Methyl 2-azido-2-methoxyacetate

HRID 1658003ノート

反応式

HRID 1658003 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 20357785Methyl 2-azido-2-methoxyacetate収率 72.4%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-4eede6886068485f9df11ad30c1b9b70
出典データセット
uspto-grants-1976_06
特許番号
US03962224

反応ノート

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