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

HRID 357482ノート

反応式

HRID 357482 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-adbef3802671476d8d696eb6b9720bf6
出典データセット
uspto-grants-1998_11
特許番号
US05840892

反応ノート

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