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2,2,6,6-Tetramethylpiperidine → HCID 21541288, 화합물

HRID 1075856
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HRID 1075856 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 21541288HCID 21541288, 화합물수율 18.9%

시약·촉매·용매 1

HCID 62761-Pentanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d651a62c6cf480d841d1c8aabbbff79
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03954776

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