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

HRID 1730640

反応式

HRID 1730640 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 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. customAfter drying phase
  5. washrepeatedly washed with water
  6. dry with materialAfter drying over Na2SO4
  7. concentrationthe solution is concentrated in vacuo

出典と根拠

ORDレコード
ord-8fc656c33893467281e6e931b34dddb2
出典データセット
uspto-grants-1976_11
特許番号
US03993655

関連ノート

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