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Hydrochloric Acid → alpha-Methyl-3(2-naphthoyl)benzene Acetic Acid

HRID 49642
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HRID 49642 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([C:13]1[CH2:14][CH2:15][CH2:16][C:17]2[C:21]=1[O:20][C:19](=[O:22])[C:18]=2[CH3:23])=[O:12].[K+].C([O-])(=O)C.C1(C)C=CC=CC=1.Cl>O>[CH3:23][CH:18]([C:17]1[CH:16]=[CH:15][CH:14]=[C:13]([C:11]([C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH:1]=2)=[O:12])[CH:21]=1)[C:19]([OH:22])=[O:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 517044Potassium AcetateHCID 129913627-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone

생성물 1

HCID 9901064alpha-Methyl-3(2-naphthoyl)benzene Acetic Acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
220 °C

실험 절차

A mixture of 7-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone (10 g) and acetic acid potassium salt (0.3 g) was added to a reactor and stirred for 1 hr at 220° C. The reaction mixture was cooled down to room temperature. Toluene and water were added to the reaction mixture and acidified to pH 2 with 5% hydrochloric acid. Toluene layer separated was dried over anhydrous MgSO4, filtered and evaporated to give crude product. The crude product was purified by column chromatograph on silica gel by eluting with a mixture of ethylacetate and n-hexane (1:5) to give the desired product (9:42 g, 94 % .

후처리

  1. additionwas added to a reactor
  2. temperatureThe reaction mixture was cooled down to room temperature
  3. customToluene layer separated
  4. dry with materialwas dried over anhydrous MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give crude product
  8. customThe crude product was purified by column chromatograph on silica gel
  9. washby eluting with a mixture of ethylacetate and n-hexane (1:5)

출처 및 근거

ORD 기록
ord-1f4befc33ffa492db518647e07a976d7
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06706917B1

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