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Triethylamine → 1-Acryloyl-2,6-diethyl-2,3,6-trimethylpiperidine

HRID 66252
ノート
印刷プレビュー

反応式

HRID 66252 の反応式
[CH2:1]([C:3]1([CH3:13])[CH:8]([CH3:9])[CH2:7][CH2:6][C:5]([CH2:11][CH3:12])([CH3:10])[NH:4]1)[CH3:2].[C:14](Cl)(=[O:17])[CH:15]=[CH2:16].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:14]([N:4]1[C:5]([CH2:11][CH3:12])([CH3:10])[CH2:6][CH2:7][CH:8]([CH3:9])[C:3]1([CH2:1][CH3:2])[CH3:13])(=[O:17])[CH:15]=[CH2:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 205360782,6-Diethyl-2,3,6-trimethylpiperidine

生成物 1

HCID 227545731-Acryloyl-2,6-diethyl-2,3,6-trimethylpiperidine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

36.7 g of 2,6-diethyl-2,3,6-trimethylpiperidine (Compound No. 1) are dissolved in 200 ml toluene. A solution of 19 g acrylic chloride in 50 ml toluene is added slowly within an hour and the mixture is stirred at 70°-75° C. for 18 hours. After addition of 21.2 g of triethylamine the stirring is continued for another 24 hours. After cooling the reaction mixture is washed twice with 100 ml water each. The toluene solution is dried over sodium sulfate and evaporated. The residue is distilled in vacuo and there is obtained the 1-acryloyl-2,6-diethyl-2,3,6-trimethylpiperidine (Compound No. 12) as distillate at 133°-135° C./0.6 mm Hg.

後処理

  1. waitis continued for another 24 hours
  2. temperatureAfter cooling the reaction mixture
  3. washis washed twice with 100 ml water each
  4. dry with materialThe toluene solution is dried over sodium sulfate
  5. customevaporated
  6. distillationThe residue is distilled in vacuo

出典と根拠

ORDレコード
ord-eb10d7c1a1e14f47b5cccd80dd7a2c25
出典データセット
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04131599

反応ノート

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