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Oxalic Acid → 2-(4,6-Dimethylpyrimidin-2-yl)oxy-3,3dimethylbutyric acid

HRID 1073026
ノート
印刷プレビュー

反応式

HRID 1073026 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([O:9][CH:10]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:11]([O:13]C)=[O:12])[N:3]=1.[OH-].[K+].C1(C)C=CC=CC=1.C(O)(=O)C(O)=O>CO.O>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([O:9][CH:10]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:11]([OH:13])=[O:12])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 971Oxalic AcidHCID 1140TolueneHCID 14797Potassium HydroxideHCID 15070275Methyl 2-(4,6-dimethylpyrimidin-2-yl)oxy3,3-dimethylbutyrate

生成物 1

HCID 150702762-(4,6-Dimethylpyrimidin-2-yl)oxy-3,3dimethylbutyric acid収率 84.7%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 962Water溶媒

実験手順

1.5 g of methyl 2-(4,6-dimethylpyrimidin-2-yl)oxy3,3-dimethylbutyrate was dissolved in 10 ml of methanol, and 10 ml of an aqueous solution containing 0.5 g of potassium hydroxide was added thereto. The mixture was stirred at room temperature for 12 hours and then shaked with 210 ml of toluene and 30 ml of water in a separatory funnel. The aqueous layer was acidified with an oxalic acid aqueous solution and extracted with 100 ml of ethyl ether. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain 1.2 g of the desired product.

後処理

  1. additionwas added
  2. extractionextracted with 100 ml of ethyl ether
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-01222139f9bc4c9bb3eb5df0f4a7f1da
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04968340

反応ノート

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