Tetrahydrofuran → HCID 68586097, 화합물

HRID 18060노트

반응식

HRID 18060 반응식
CS(C[C:6]1[CH:7]=[C:8]([CH2:12][OH:13])[CH:9]=[CH:10][CH:11]=1)(=O)=O.[CH3:14][S:15](CC1C=C(C=CC=1)C(O)=O)(=[O:17])=[O:16].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].O1CCC[CH2:37]1>O.C(OCC)(=O)C>[CH3:14][S:15]([C:6]1[C:7]([CH3:37])=[C:8]([CH2:12][OH:13])[CH:9]=[CH:10][CH:11]=1)(=[O:17])=[O:16]

참가 물질

8

반응물 5

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 49625833-(Methanesulfonylmethyl)benzoic acidHCID 17908456HCID 17908456, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 68586097HCID 68586097, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

(3-Methylsulfonylmethylphenyl)methanol may be prepared by carrying out the procedure in the following manner: a mixture of 26 g of 3-(methylsulfonylmethyl)-benzoic acid and 4.6 g of lithium aluminum hydride in 600 cm3 of tetrahydrofuran is stirred for 18 hours at a temperature close to 20° C. The solution is cooled to 0° C. and then 15 cm3 of ethyl acetate, 30 cm3 of water, 5 cm3 of a 15% aqueous solution of sodium hydroxide and finally 30 cm3 of water are added-successively. The mixture is filtered on celite and the filtrate taken up in 600 cm3 of ethyl acetate. The organic phase is taken up in 500 cm3 of water and then 200 cm3 of a saturated aqueous sodium chloride solution, separated after settling, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness under reduced pressure (2.7 kPa). 10.4 g of (3-methylsulfonyl-methylphenyl)methanol are obtained in the form of a gum.

후처리

  1. customclose to 20° C
  2. filtrationThe mixture is filtered on celite
  3. custom200 cm3 of a saturated aqueous sodium chloride solution, separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

출처 및 근거

ORD 기록
ord-1b6b0f04f21e4f3b97941b6a3249547d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741316B2

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