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

HRID 847669노트

반응식

HRID 847669 반응식
[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>[CH2:12]([C:3]([CH2:1][CH3:2])([C:8]([O:10][CH:11]1[CH2:27][C:18]([CH3:19])([CH3:26])[N:17]([CH2:14][CH:15]=[CH2:16])[C:22]([CH3:21])([CH3:23])[CH2:24]1)=[O:9])[C:4]([O:6][CH:7]1[CH2:24][C:22]([CH3:23])([CH3:21])[N:17]([CH2:14][CH:15]=[CH2:16])[C:18]([CH3:27])([CH3:26])[CH2:19]1)=[O:5])[CH3:13]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-9880888cada64eb0b2423ff6cef9425a
출처 데이터셋
uspto-grants-1981_10
특허 번호
US04293468

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