Acetic Acid → beta-Methoxy-beta-(3-nitro-2,4,6-trimethylphenylhydrazino)-acrylic acid ethyl ester

HRID 2398926노트

반응식

HRID 2398926 반응식
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]([O:11][CH3:12])(OC)OC)[CH3:2].C(O)(=O)C.[N+:18]([C:21]1[C:22]([CH3:31])=[C:23]([NH:29][NH2:30])[C:24]([CH3:28])=[CH:25][C:26]=1[CH3:27])([O-:20])=[O:19]>CO>[CH2:1]([O:3][C:4](=[O:13])[CH:5]=[C:6]([O:11][CH3:12])[NH:30][NH:29][C:23]1[C:24]([CH3:28])=[CH:25][C:26]([CH3:27])=[C:21]([N+:18]([O-:20])=[O:19])[C:22]=1[CH3:31])[CH3:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 19938995HCID 19938995, 화합물HCID 214319753-Nitro-2,4,6-trimethylphenylhydrazine

생성물 1

HCID 86734787beta-Methoxy-beta-(3-nitro-2,4,6-trimethylphenylhydrazino)-acrylic acid ethyl ester수율 37.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

26.9 g (0.14 mol) of trimethoxypropionic acid ethyl ester (prepared according to DT-OS 2,042,920 ) are dissolved in 100 ml of absolute methanol, 7 ml of glacial acetic acid are added and the mixture is heated to the boil. 23.4 g (0.12 mol) of 3-nitro-2,4,6-trimethylphenylhydrazine (prepared according to DT-OS 2,156,913) are introduced in portions into the mixture over the course of 10 minutes. The mixture is stirred for a further 10 minutes at the boil and is allowed to cool whilst stirring. The orange crystals which have precipitated are filtered off, washed with a little methanol and dried (18 hours in vacuo at 50° C.). 14.4 g of β-methoxy-β-(3-nitro-2,4,6-trimethylphenylhydrazino)-acrylic acid ethyl ester of melting point 82° - 83° C. are obtained.

후처리

  1. temperaturethe mixture is heated to the boil
  2. temperatureto cool
  3. stirringwhilst stirring
  4. customThe orange crystals which have precipitated
  5. filtrationare filtered off
  6. washwashed with a little methanol
  7. customdried (18 hours in vacuo at 50° C.)

출처 및 근거

ORD 기록
ord-cdbbb438b1724c988fce83aac6e98ad7
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04026709

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