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Water → HCID 19366807, 화합물

HRID 849532
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HRID 849532 반응식
C[CH:2]([CH:6]([S:8]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)(=[O:10])=[O:9])[CH3:7])[C:3](O)=[O:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH3:18][O:17][C:14]1[CH:13]=[CH:12][C:11]([S:8]([CH:6]([CH3:7])[CH2:2][CH2:3][OH:4])(=[O:9])=[O:10])=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 19366821HCID 19366821, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19366807HCID 19366807, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Part B: To a solution of 3.5 g (13 mmol) of methyl 3-[(4-methoxyphenyl)sulfonyl]-butanoic acid from Part A in 50 mL of anhydrous THF at zero° C. under nitrogen, was added 14.2 mL (0.5 g, 13 mmol) of a 1.0 M solution of lithium aluminum hydride in THF. After 1.5 hours, the reaction mixture was cooled to zero° C. and z0.6 mL of water was added, followed by 0.6 mL of 2.5 N sodium hydroxide solution and 1.8 mL of water, the reaction was filtered, the filtrate concentrated in vacuo, ethyl acetate and 5% citric acid solution were added, the organic layer was separated and washed with saturated sodium bicarbonate solution and brine, dried with magnesium sulfate, filtered and concentrated to afford 2.7 grams of pure 3-[(4-methoxyphenyl)-sulfonyl]butan-1-ol, m/z=251 (M+Li).

후처리

  1. temperaturethe reaction mixture was cooled
  2. filtrationthe reaction was filtered
  3. concentrationthe filtrate concentrated in vacuo, ethyl acetate and 5% citric acid solution
  4. additionwere added
  5. customthe organic layer was separated
  6. washwashed with saturated sodium bicarbonate solution and brine
  7. dry with materialdried with magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-88a3cef68c2f43c9bb72c62c3f7c77a9
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06013649

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