Acetic Anhydride → alpha-Nitro-beta-ethoxyacrylic acid methylester

HRID 616263

反応式

HRID 616263 の反応式
[CH3:1][O:2][C:3](=[O:8])[CH2:4][N+:5]([O-:7])=[O:6].[CH:9](OCC)(OCC)[O:10][CH2:11][CH3:12].C(OC(=O)C)(=O)C>>[CH3:1][O:2][C:3](=[O:8])[C:4]([N+:5]([O-:7])=[O:6])=[CH:9][O:10][CH2:11][CH3:12]

参加物

4

反応物 3

HCID 7918Acetic AnhydrideHCID 17206Methyl 2-nitroacetateHCID 31214Ethyl orthoformate

生成物 1

HCID 53395203alpha-Nitro-beta-ethoxyacrylic acid methylester収率 84.5%

実験手順

A 12-l. three-necked flask, equippedewith a thermometer, mechanical stirrer and a reflux condenser was charged under an atmosphere of nitrogen with 746 g (6.26 moles) of nitroacetic acid methylester, 1392 g (9.4 moles) of triethyl orthoformate and 1.92 l of acetic anhydride. The mixture was stirred and heated at reflux for 23 hours. The volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C, then at aspirator; vacuum and finally at 0.17 mmHg, (pot temperature up to 70°), leaving 926 g (84%) of crude alpha-nitro-beta-ethoxyacrylic acid methylester as an orange oil.

後処理

  1. temperatureheated
  2. temperatureat reflux for 23 hours
  3. distillationThe volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C

出典と根拠

ORDレコード
ord-f7396bc9f65f41088d8d53343f8429c9
出典データセット
uspto-grants-1978_02
特許番号
US04073795

関連ノート

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