Potassium Carbonate → tert-Butyl[4-(7-chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

HRID 633616ノート

反応式

HRID 633616 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:9]2[N:18]=[C:17]([C:19]3[CH:24]=[C:23]([CH3:25])[C:22]([OH:26])=[C:21]([CH3:27])[CH:20]=3)[O:16][C:10]=2[N:11]=[C:12]([S:14][CH3:15])[N:13]=1.Br[CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31]>CN(C)C=O>[Cl:7][C:8]1[C:9]2[N:18]=[C:17]([C:19]3[CH:24]=[C:23]([CH3:25])[C:22]([O:26][CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])=[C:21]([CH3:27])[CH:20]=3)[O:16][C:10]=2[N:11]=[C:12]([S:14][CH3:15])[N:13]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79177tert-Butyl bromoacetateHCID 1364132354-(7-Chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenol

生成物 1

HCID 89350956tert-Butyl[4-(7-chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

7.46 g of potassium carbonate were added to a solution of 4.34 g of 4-(7-chloro-5-methylsulfanyloxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenol in 45 ml of dimethylformamide, and 2.90 g of tert-butyl bromoacetate were then added. The mixture was stirred at 60° C. for 1 h. The cooled reaction mixture was then added to ice water, and the precipitated solid was filtered off with suction and washed with water. The solid was taken up in dichloromethane and dried over sodium sulfate, activated carbon was added and the mixture was filtered and concentrated under reduced pressure. This gave 4.20 g (71%) of the title compound, which was reacted further without any further purification.

後処理

  1. additionwere then added
  2. customThe cooled reaction mixture
  3. filtrationthe precipitated solid was filtered off with suction
  4. washwashed with water
  5. dry with materialdried over sodium sulfate, activated carbon
  6. additionwas added
  7. filtrationthe mixture was filtered
  8. concentrationconcentrated under reduced pressure
  9. customThis gave 4.20 g (71%) of the title compound, which was reacted further without any further purification

出典と根拠

ORDレコード
ord-13169866d1014eb9a6548b35d9ea6f12
出典データセット
uspto-grants-2016_04
特許番号
US09321787B2

反応ノート

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