Hydrazine hydrate (1:1) → 3-(4-Hydroxy-3-methylbenzofuran-2-yl)propionic acid

HRID 978120노트

반응식

HRID 978120 반응식
[OH:1][C:2]1[C:7]2[C:8]([CH3:16])=[C:9](/[CH:11]=[CH:12]/[C:13]([OH:15])=[O:14])[O:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.O.NN>O.S([O-])([O-])(=O)=O.[Cu+2].CO>[OH:1][C:2]1[C:7]2[C:8]([CH3:16])=[C:9]([CH2:11][CH2:12][C:13]([OH:15])=[O:14])[O:10][C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 13849550E-3-(4-hydroxy-3-methylbenzofuran-2-yl)propenoic acid

생성물 1

HCID 138495513-(4-Hydroxy-3-methylbenzofuran-2-yl)propionic acid수율 21.6%

시약·촉매·용매 2

HCID 61499Cupric sulfate monohydrate촉매HCID 887Methanol용매

실험 절차

A mixture of E-3-(4-hydroxy-3-methylbenzofuran-2-yl)propenoic acid (4.5 g, 20 mmoles), methanol (250 ml), 99% hydrazine hydrate (5 ml) and copper sulfate monohydrate (3 crystals) was stirred at room temperature for several days. The mixture was filtered and concentrated to remove methanol. The aqueous residue was acidified with 20% citric acid solution and extracted with diethyl ether. The ether solution was dried with Na2SO4, filtered, concentrated and chromatographed to obtain 950 mg of the title compound, m.p. 114°-117° C.

후처리

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customto remove methanol
  4. extractionextracted with diethyl ether
  5. dry with materialThe ether solution was dried with Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customchromatographed

출처 및 근거

ORD 기록
ord-66a8950cc8004c1da350a0eed19877a3
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04663347

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