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Lithium Hydroxide → (2E)-3-[4-(Methylsulfonyl)phenyl]propenoic acid

HRID 2212031
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반응식

HRID 2212031 반응식
C([O:3][C:4](=[O:17])/[CH:5]=[CH:6]/[C:7]1[CH:12]=[CH:11][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9][CH:8]=1)C.[OH-].[Li+]>O1CCOCC1.O>[CH3:16][S:13]([C:10]1[CH:11]=[CH:12][C:7](/[CH:6]=[CH:5]/[C:4]([OH:17])=[O:3])=[CH:8][CH:9]=1)(=[O:14])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 10634688HCID 10634688, 화합물

생성물 1

HCID 5702855(2E)-3-[4-(Methylsulfonyl)phenyl]propenoic acid

시약·촉매·용매 1

HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

A solution of (E)-3-(4-(methylsulfonyl)phenyl)acrylic acid ethyl ester and lithium hydroxide in dioxane/water (100 ml/100 ml) was stirred for 16 h at room temp. It was washed with tert.-butyl methyl ether (200 ml). The aqueous phase was acidified with a 10% aqueous solution of sodium hydrogensulfate until pH 2. The precipitation was isolated by filtration and dried in vacuo. The residue was suspended in ethanol (100 ml). The solvent was removed. The latter procedure was repeated once to give 2.74 g of crude (E)-4-methylsulfonylcinnamic acid which was used in the next step without further purification.

후처리

  1. washIt was washed with tert.-butyl methyl ether (200 ml)
  2. customThe precipitation
  3. customwas isolated by filtration
  4. customdried in vacuo
  5. customThe solvent was removed

출처 및 근거

ORD 기록
ord-c2645ec8cac940c7bc5fe40dcdf5aa16
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07101898B2

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