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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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p-Toluenesulfonic acid monohydrate → 4-Methoxy-4-(methoxymethyl)cyclohexanone

HRID 922121
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HRID 922121 반응식
[CH3:1][O:2][C:3]1([CH2:13][O:14][CH3:15])[CH2:12][CH2:11][C:6]2(OCC[O:7]2)[CH2:5][CH2:4]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O.O>[CH3:1][O:2][C:3]1([CH2:13][O:14][CH3:15])[CH2:4][CH2:5][C:6](=[O:7])[CH2:11][CH2:12]1
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참가 물질

5

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 712474008-Methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane

생성물 1

HCID 857431314-Methoxy-4-(methoxymethyl)cyclohexanone

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

13.3 g (61.5 mmol) of the compound from Example 10A were dissolved in 200 ml of acetone and 100 ml of water, 1.87 g (9.84 mmol) of 4-toluenesulphonic acid monohydrate were added and the mixture was stirred at room temperature for two days. The acetone was then distilled off, the aqueous residue was neutralized by addition of sodium bicarbonate and 23.2 g of sodium chloride were added. The mixture was extracted repeatedly with ethyl acetate and the combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulphate, filtered and concentrated. This gave 10.3 g (97% of theory) of the title compound.

후처리

  1. distillationThe acetone was then distilled off
  2. additionthe aqueous residue was neutralized by addition of sodium bicarbonate and 23.2 g of sodium chloride
  3. additionwere added
  4. extractionThe mixture was extracted repeatedly with ethyl acetate
  5. washthe combined organic phases were washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5620cb49020c45ec96805aaef14feff6
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278925B2

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