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

HRID 2398926ノート

反応式

HRID 2398926 の反応式
[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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 19938995HCID 19938995、化合物HCID 214319753-Nitro-2,4,6-trimethylphenylhydrazine

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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.)

出典と根拠

ORDレコード
ord-cdbbb438b1724c988fce83aac6e98ad7
出典データセット
uspto-grants-1977_05
特許番号
US04026709

反応ノート

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