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Lithium Hydroxide → HCID 22218187, 화합물

HRID 1602863
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HRID 1602863 반응식
[CH3:1][S:2]([CH2:5][C:6](=[CH2:11])[C:7]([O:9]C)=[O:8])(=[O:4])=[O:3].[OH-].[Li+].S([O-])(O)(=O)=O.[K+]>O1CCCC1.O>[CH3:1][S:2]([CH2:5][C:6](=[CH2:11])[C:7]([OH:9])=[O:8])(=[O:4])=[O:3]
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참가 물질

6

반응물 3

HCID 3939Lithium HydroxideHCID 516920Potassium bisulfateHCID 22218188Methyl 2-(methylsulfonylmethyl)acrylate

생성물 1

HCID 22218187HCID 22218187, 화합물수율 89%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of methyl 2-(methylsulfonylmethyl)acrylate (970 mg, 5.44 mmol) in 15 mL of tetrahydrofuran was treated with a solution of lithium hydroxide (270 mg, 6.4 mmol) in 7 mL of water. The solution was stirred at room temperature for 5 m and then acidified to pH=1 with 1 N aqueous potassium hydrogen sulfate and the solution extracted three times with ethyl acetate. The combined ethyl acetate solution was dried over anhydrous magnesium sulfate, filtered, and concentrated to give 793 mg, 89% of 2-(methylsulfonylmethyl) acrylic acid, mp 147-149 0° C.

후처리

  1. extractionthe solution extracted three times with ethyl acetate
  2. dry with materialThe combined ethyl acetate solution was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-416d7bb28c8e404d838f59c642644101
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05985870

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