Potassium Carbonate → HCID 86679897, 화합물

HRID 403465

반응식

HRID 403465 반응식
[C:1]([O:5][C:6](=[O:34])[CH2:7][O:8][C:9]1[C:14]([CH3:15])=[CH:13][C:12]([C:16]2[O:17][C:18]3[N:19]=[C:20](S(C)(=O)=O)[N:21]=[C:22]([O:25][CH2:26][CH2:27][CH3:28])[C:23]=3[N:24]=2)=[CH:11][C:10]=1[CH3:33])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[F:41][C:42]1[CH:47]=[CH:46][C:45]([F:48])=[CH:44][C:43]=1[OH:49].S([O-])(O)(=O)=O.[Na+]>CN(C)C=O>[C:1]([O:5][C:6](=[O:34])[CH2:7][O:8][C:9]1[C:14]([CH3:15])=[CH:13][C:12]([C:16]2[O:17][C:18]3[N:19]=[C:20]([O:49][C:43]4[CH:44]=[C:45]([F:48])[CH:46]=[CH:47][C:42]=4[F:41])[N:21]=[C:22]([O:25][CH2:26][CH2:27][CH3:28])[C:23]=3[N:24]=2)=[CH:11][C:10]=1[CH3:33])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 949522,5-DifluorophenolHCID 516919Sodium BisulfateHCID 86679896Tert-butyl [4-(5-methanesulfonyl-7-propoxyoxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

생성물 1

HCID 86679897HCID 86679897, 화합물수율 62.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 100 mg [4-(5-methanesulfonyl-7-propoxy-oxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethyl-phenoxy]-acetic acid tert-butyl ester in 1.5 ml of N,N-dimethylformamide were added 62 mg of potassium carbonate and 32 mg of 2,5-difluoro-phenol. The mixture was stirred at room temperature for 12 h. Then the mixture was poured onto water, neutralized by addition of a 10% aqueous solution of sodium hydrogensulfate, and extracted twice with ethyl acetate. The combined organic layers were dried and concentrated in vacuo. After filtration the solvent was distilled off in vacuo and the residue purified by preparative HPLC to yield 69 mg of the title compound.

후처리

  1. additionThen the mixture was poured onto water
  2. extractionextracted twice with ethyl acetate
  3. customThe combined organic layers were dried
  4. concentrationconcentrated in vacuo
  5. filtrationAfter filtration the solvent
  6. distillationwas distilled off in vacuo
  7. customthe residue purified by preparative HPLC

출처 및 근거

ORD 기록
ord-586565833103405e8359d34c96995918
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748436B2

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