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

HRID 127497

반응식

HRID 127497 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 53395203alpha-Nitro-beta-ethoxyacrylic acid methylester수율 84.5%

실험 절차

A 12-1. three-necked flask, equipped with 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.

후처리

  1. customthree-necked flask, equipped with a thermometer, mechanical stirrer and a reflux condenser
  2. temperatureheated
  3. temperatureat reflux for 23 hours
  4. distillationThe volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C.

출처 및 근거

ORD 기록
ord-f4cc5be488af4ae89d3ca1bd70b19add
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256641

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