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2,2,6,6-Tetramethylpiperidine → HCID 21541288、化合物

HRID 1075856
ノート
印刷プレビュー

反応式

HRID 1075856 の反応式
[CH3:1][C:2]1([CH3:10])[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[NH:3]1.[O:11]1[CH:13]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)[CH:17]=2)[CH2:12]1>CCCCCO>[CH3:1][C:2]1([CH3:10])[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[N:3]1[CH2:12][CH:13]([OH:11])[CH2:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 130352,2,6,6-TetramethylpiperidineHCID 129198521,2-Epoxy-3-[3-(2-pyridylmethyl)phenoxy]propane

生成物 1

HCID 21541288HCID 21541288、化合物収率 18.9%

試薬・触媒・溶媒 1

HCID 62761-Pentanol溶媒

実験手順

8.9 g of 2,2,6,6-tetramethylpiperidine is added to a solution of 15.0 g of 1,2-epoxy- 3-[3-(2-pyridylmethyl)phenoxy]propane in 45 ml of n-amyl alcohol, and the resulting mixture is heated on a water bath for 2 hours. The solvent is then removed, 200 ml of benzene is added to the residue, and the insoluble matter is filtered off with activated charcoal. The filtrate is washed with water, and extracted with two 100 ml portions of 5% hydrochloric acid. The aqueous layer is made alkaline with sodium hydroxide, and the separated oil is extracted with benzene. The benzene layer is washed with water, dried over anhydrous potassium carbonate, and the solvent is removed. The residual oil is purified by distillation to give 4.5 g of 1-(2,2,6,6-tetramethylpiperidino)-3-[3-(2-pyridylmethyl)phenoxy]-2 -propanol, boiling at 230°-235°C/0.15 mmHg.

後処理

  1. temperaturethe resulting mixture is heated on a water bath for 2 hours
  2. customThe solvent is then removed
  3. addition200 ml of benzene is added to the residue
  4. filtrationthe insoluble matter is filtered off with activated charcoal
  5. washThe filtrate is washed with water
  6. extractionextracted with two 100 ml portions of 5% hydrochloric acid
  7. extractionthe separated oil is extracted with benzene
  8. washThe benzene layer is washed with water
  9. dry with materialdried over anhydrous potassium carbonate
  10. customthe solvent is removed
  11. distillationThe residual oil is purified by distillation

出典と根拠

ORDレコード
ord-1d651a62c6cf480d841d1c8aabbbff79
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03954776

反応ノート

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