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Benzophenone → (2,6-Difluorophenyl)(4-methoxyphenyl)methanone

HRID 974117
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HRID 974117 반응식
FC1C=CC=C(F)C=1C(Cl)=O.C1(OC)C=CC=CC=1.C(C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(O)C#C.C1C=CC2C(=CC=CC=2O)C=1.[OH-].[Na+].[F:51][C:52]1[CH:57]=[CH:56][CH:55]=[C:54]([F:58])[C:53]=1[C:59]1([C:73]2[CH:78]=[CH:77][C:76]([O:79][CH3:80])=[CH:75][CH:74]=2)[O:64]C2C=CC3C(C=2C=C1)=CC=CC=3>C(=S)=S.[Cl-].[Al+3].[Cl-].[Cl-].C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[F:51][C:52]1[CH:57]=[CH:56][CH:55]=[C:54]([F:58])[C:53]=1[C:59]([C:73]1[CH:74]=[CH:75][C:76]([O:79][CH3:80])=[CH:77][CH:78]=1)=[O:64]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 7

HCID 3102BenzophenoneHCID 70051-NaphtholHCID 7519AnisoleHCID 7859Propargyl alcohol2회HCID 14798Sodium HydroxideHCID 874382,6-Difluorobenzoyl chlorideHCID 214667653-(2,6-Difluorophenyl)-3-(4-methoxyphenyl)-3H-naphtho[2,1-b]pyran

생성물 1

HCID 19987799(2,6-Difluorophenyl)(4-methoxyphenyl)methanone

시약·촉매·용매 4

HCID 6101p-Toluenesulfonic acid촉매HCID 6451240Aluminum(III) Chloride촉매HCID 241Benzene용매2회HCID 6348Carbon Disulfide용매

실험 절차

2,6-difluoro-4'-methoxybenzophenone was prepared by Friedel-Crafts reaction of 2,6-difluorobenzoyl chloride with anisole in carbon disulfide using aluminum chloride as catalyst. 4.8 grams (0.02 mole) of the benzophenone was converted to the propargyl alcohol using the conditions described in Example 1, Step 2. The crude propargyl alcohol was taken up in 200 milliliters of benzene and 3.0 grams (0.02 mole) of naphthol and 0.1 grams of p-toluene sulfonic acid catalyst was added to the benzene solution. After stirring for 1 hour, the reaction mixture was poured into an equal volume of 5 percent aqueous sodium hydroxide. The organic layer was separated and the benzene solvent removed on a rotary evaporator. The residue was chromatographed on silica using a 4:1 mixture of hexane:ethyl acetate as elutant. The photochromic fractions were collected and crystallized from n-propanol. 1.2 grams of product having a melting range of 122-124° C. was obtained. NMR analysis confirmed the product to be 3(2,6-difluorophenyl)-3(4-methoxyphenyl)-3H- naphtho[ 2,1-b]pyran.

후처리

  1. customThe organic layer was separated
  2. customthe benzene solvent removed on a rotary evaporator
  3. customThe residue was chromatographed on silica using
  4. additiona 4:1 mixture of hexane
  5. customThe photochromic fractions were collected
  6. customcrystallized from n-propanol
  7. customwas obtained

출처 및 근거

ORD 기록
ord-e7725307cd854309a1623013337b2a60
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05066818

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