Potassium Carbonate → Methyl (+/-)-2-(4,6-dimethoxy-2-pyrimidinyloxy)-3,3-dimethylbutanoate

HRID 357482노트

반응식

HRID 357482 반응식
[CH3:1][O:2][CH:3]1[C:8](=S(=O)=O)[C:7]([O:12][CH3:13])=[N:6][C:5](C)=[N:4]1.[OH:15][CH:16]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:17]([O:19][CH3:20])=[O:18].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:12][CH3:13])[N:6]=[C:5]([O:15][CH:16]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:17]([O:19][CH3:20])=[O:18])[N:4]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 9855510Methyl 2-hydroxy-3,3-dimethylbutanoateHCID 771347914,6-Dimethoxy-2-methyl-sulfonylpyrimidine

생성물 1

HCID 11011508Methyl (+/-)-2-(4,6-dimethoxy-2-pyrimidinyloxy)-3,3-dimethylbutanoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.18 g (10.0 mmol) of 4,6-dimethoxy-2-methyl-sulfonylpyrimidine and 1.62 g (11.0 mmol) of methyl (+/-)-2-hydroxy-3,3-dimethylbutanoate were heated in the presence of 2.07 g (15.0 mmol) of potassium carbonate in 20 ml of N,N-dimethylformamide to 60° with stirring. After 3 hours, the solvent was removed in a rotary evaporator at 60° C./20 mbar. The residue was taken up in 40 ml of water and 40 ml of ethyl acetate. After the organic phase had been separated off, the aqueous phase was again extracted with 40 ml of ethyl acetate. The combined organic phases was washed with water, dried over magnesium sulfate and evaporated. The title product was obtained in a yield of 2.76 g (93.8 percent of theory) in the form of pale yellowish crystals (GC content 96.6 percent).

후처리

  1. customthe solvent was removed in a rotary evaporator at 60° C./20 mbar
  2. customAfter the organic phase had been separated off
  3. extractionthe aqueous phase was again extracted with 40 ml of ethyl acetate
  4. washThe combined organic phases was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-adbef3802671476d8d696eb6b9720bf6
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840892

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