Dimethyl diethylmalonate → Bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate

HRID 1164387ノート

反応式

HRID 1164387 の反応式
[CH2:1]([C:3]([CH2:12][CH3:13])([C:8]([O:10][CH3:11])=[O:9])[C:4]([O:6][CH3:7])=[O:5])[CH3:2].[CH2:14]([N:17]1[C:22]([CH3:24])([CH3:23])[CH2:21]C(O)[CH2:19][C:18]1([CH3:27])[CH3:26])[CH:15]=[CH2:16]>C1(C)C(C)=CC=CC=1>[CH2:14]([N:17]1[C:22]([CH3:24])([CH3:23])[CH2:21][CH:7]([O:6][C:4](=[O:5])[C:3]([CH2:1][CH3:2])([CH2:12][CH3:13])[C:8]([O:10][CH:11]2[CH2:27][C:18]([CH3:19])([CH3:26])[N:17]([CH2:14][CH:15]=[CH2:16])[C:22]([CH3:21])([CH3:23])[CH2:24]2)=[O:9])[CH2:19][C:18]1([CH3:27])[CH3:26])[CH:15]=[CH2:16]

参加物

4

反応物 2

HCID 117935Dimethyl diethylmalonateHCID 129919752,2,6,6-Tetramethyl-1-(prop-2-en-1-yl)piperidin-4-ol

生成物 1

HCID 20512150Bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

After the addition of 1 g of tetrabutyl-orthotitanate, 47 g of dimethyl diethylmalonate and 98.6 g of 1-allyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 100 ml of xylene are heated under a gentle stream of nitrogen to about 140°. The methanol forming during the reaction is continuously distilled off, and after about 6 hours the reaction is virtually completed. The reaction mixture is diluted with 200 ml of toluene, extracted three times with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from hexane yields bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl)diethylmalonate (compound 18), m.p. 135°-136°.

後処理

  1. temperatureare heated under a gentle stream of nitrogen to about 140°
  2. distillationThe methanol forming during the reaction is continuously distilled off
  3. additionThe reaction mixture is diluted with 200 ml of toluene
  4. extractionextracted three times with 100 ml of water each time
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated by evaporation
  7. customCrystallisation of the residue from hexane

出典と根拠

ORDレコード
ord-6d5d6371dd0049b9a5efb068eee4ce36
出典データセット
uspto-grants-1983_01
特許番号
US04369275

反応ノート

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