Potassium Carbonate → Ethyl 3-[3-tert-butyl-4-(2-{4-[(methylsulfonyl)oxy]phenyl}ethoxy)phenyl]-2-ethoxypropanoate

HRID 353300

반응식

HRID 353300 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH2:12][CH:13]([O:19][CH2:20][CH3:21])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:8]=[CH:9][C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[CH3:22][S:23]([O:26][C:27]1[CH:32]=[CH:31][C:30]([CH2:33][CH2:34]OS(C)(=O)=O)=[CH:29][CH:28]=1)(=[O:25])=[O:24].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[C:1]([C:5]1[CH:6]=[C:7]([CH2:12][CH:13]([O:19][CH2:20][CH3:21])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:8]=[CH:9][C:10]=1[O:11][CH2:34][CH2:33][C:30]1[CH:29]=[CH:28][C:27]([O:26][S:23]([CH3:22])(=[O:24])=[O:25])=[CH:32][CH:31]=1)([CH3:2])([CH3:4])[CH3:3]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 112201221-(Methylsulfonyloxy)-2-[4-(methylsulfonyloxy)phenyl]ethaneHCID 22708416Ethyl 3-(3-tert-butyl-4-hydroxyphenyl)-2-ethoxypropanoate

생성물 1

HCID 10300195Ethyl 3-[3-tert-butyl-4-(2-{4-[(methylsulfonyl)oxy]phenyl}ethoxy)phenyl]-2-ethoxypropanoate수율 22.1%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

Ethyl 3-(3-tert-butyl-4-hydroxyphenyl)-2-ethoxypropanoate (0.15 g, 0.44 mmole) and 4-{2-[(methylsulfonyl)oxy]ethyl}phenyl methanesulfonate (0.26 g, 0.89 mmole) were dissolved in 2-butanone (4 ml). Polyethyleneglycol 400 (0.05 g) and anhydrous potassium carbonate (0.092 g, 0.67 mmole) were added the mixture. After stirring at reflux for 16 hours it was checked using HPLC whether all the starting material was consumed. The mixture was washed with water dried with magnesium sulfate and evaporated. Purification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm) using actonitrile(40-80%) in ammonium acetate buffer (pH 7) as mobile phase gave 0.048 g (22% yield) of the desired product

후처리

  1. temperatureat reflux for 16 hours it
  2. customwas consumed
  3. washThe mixture was washed with water
  4. dry with materialdried with magnesium sulfate
  5. customevaporated
  6. customPurification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm)

출처 및 근거

ORD 기록
ord-4cada9979f354ec8bfeed55abff49f4d
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750252B2

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