Acetic Acid → 3,5-Di-tert.butyl-4-hydroxybenzyl-malonic acid-bis(2,2,6,6-tetramethyl-4-piperidinyl)ester

HRID 27349

反応式

HRID 27349 の反応式
[C:1]([O:17][CH:18]1[CH2:23][C:22]([CH3:25])([CH3:24])[NH:21][C:20]([CH3:27])([CH3:26])[CH2:19]1)(=[O:16])[CH2:2][C:3]([O:5][CH:6]1[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9][C:8]([CH3:15])([CH3:14])[CH2:7]1)=[O:4].[C:28]([C:32]1[CH:33]=[C:34]([CH:39]=[C:40]([C:43]([CH3:46])([CH3:45])[CH3:44])[C:41]=1[OH:42])[CH2:35]N(C)C)([CH3:31])([CH3:30])[CH3:29].[NH2-].[Li+].C(O)(=O)C>C1(C)C=CC=CC=1>[CH3:14][C:8]1([CH3:15])[CH2:7][CH:6]([O:5][C:3](=[O:4])[CH:2]([CH2:35][C:34]2[CH:33]=[C:32]([C:28]([CH3:29])([CH3:31])[CH3:30])[C:41]([OH:42])=[C:40]([C:43]([CH3:46])([CH3:45])[CH3:44])[CH:39]=2)[C:1]([O:17][CH:18]2[CH2:23][C:22]([CH3:25])([CH3:24])[NH:21][C:20]([CH3:27])([CH3:26])[CH2:19]2)=[O:16])[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9]1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 24532Lithium amideHCID 66609Phenol, 4-[(dimethylamino)methyl]-2,6-bis(1,1-dimethylethyl)-HCID 1244568Bis(2,2,6,6-tetramethylpiperidin-4-yl) propanedioate

生成物 1

HCID 140938763,5-Di-tert.butyl-4-hydroxybenzyl-malonic acid-bis(2,2,6,6-tetramethyl-4-piperidinyl)ester

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

26 g (0.068 mole) of bis-(2,2,6,6-tetramethyl-4-piperidinyl) malonate and 17.8 g (0.068 mole) of N-(3,5-di-tert.butyl-4-hydroxybenzyl)dimethylamine are dissolved in 200 ml of toluene. After the addition of 0.5 g of lithium amide, the mixture is refluxed for 3 hours. After cooling, the mixture is neutralised with 1.5 ml of 1% acetic acid, and the organic phase repeatedly washed with water. After drying over Na2SO4, the solution is concentrated in vacuo to obtain, as oily residue, 3,5-di-tert.butyl-4-hydroxybenzyl-malonic acid-bis(2,2,6,6-tetramethyl-4-piperidinyl)ester.

後処理

  1. temperaturethe mixture is refluxed for 3 hours
  2. temperatureAfter cooling
  3. washthe organic phase repeatedly washed with water
  4. dry with materialAfter drying over Na2SO4
  5. concentrationthe solution is concentrated in vacuo

出典と根拠

ORDレコード
ord-a6dd02c1463b481ca35a80ea5c2279cf
出典データセット
uspto-grants-1980_09
特許番号
US04221701

関連ノート

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