Potassium Carbonate → HCID 15611948、化合物

HRID 357486

反応式

HRID 357486 の反応式
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[N:3]=1.[OH:12][C:13]1[C:22]([CH3:23])=[CH:21][CH:20]=[CH:19][C:14]=1[C:15]([O:17][CH3:18])=[O:16].CS([O-])=O.[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:11][O:10][C:4]1[CH:5]=[C:6]([O:8][CH3:9])[N:7]=[C:2]([O:12][C:13]2[C:22]([CH3:23])=[CH:21][CH:20]=[CH:19][C:14]=2[C:15]([O:17][CH3:18])=[O:16])[N:3]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 31835Benzoic acid, 2-hydroxy-3-methyl-, methyl esterHCID 2733271Sodium methanesulfinateHCID 51523232-Chloro-4,6-dimethoxypyrimidine

生成物 1

HCID 15611948HCID 15611948、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.38 g (25 mmol) of 2-chloro-4,6-dimethoxypyrimidine, 4.17 g (25.0 mmol) of methyl 2-hydroxy-3-methylbenzoate and 0.66 g (6.3 mmol) of sodium methanesulfinate were heated in the presence of 5.17 g (37.5 mmol) of potassium carbonate in 25 ml of N,N-dimethylformamide to 120° C. with stirring. After 8 hours, the solvent was removed in a rotary evaporator at 60° C./20 mbar. The residue was taken up in 30 ml of water and 30 ml of dichloromethane. After the organic phase had been separated off, the aqueous phase was again extracted with 20 ml of dichloromethane. The combined organic phases was washed with water, dried over magnesium sulfate and evaporated. The residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1). The title product was obtained from the product fraction in a yield of 5.23 g (65.8 percent of theory) (GC content 96 percent). The melting point of the compound was 73.8° to 79.1° C. Other data concerning the title compound was:

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 20 ml of dichloromethane
  4. washThe combined organic phases was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1)

出典と根拠

ORDレコード
ord-aefd827c51644e598e3a91380a52eda0
出典データセット
uspto-grants-1998_11
特許番号
US05840892

関連ノート

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