Methyl pivaloylacetate → HCID 178441204、化合物

HRID 617781

反応式

HRID 617781 の反応式
[CH3:1][C:2]([CH3:11])([CH3:10])[C:3](=O)[CH2:4][C:5](OC)=[O:6].C(=O)(O)O.[NH2:16][C:17]([NH2:19])=[NH:18]>C(O)C>[NH2:19][C:17]1[N:18]=[C:5]([OH:6])[CH:4]=[C:3]([C:2]([CH3:11])([CH3:10])[CH3:1])[N:16]=1

参加物

4

反応物 2

HCID 99597Methyl pivaloylacetateHCID 286947Carbonic acid-guanidine (1:1)

生成物 1

HCID 178441204HCID 178441204、化合物収率 75.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Methyl 4,4-dimethyl-3-oxopentanoate (15.82 g) and guanidine carbonate (20.0 g) were mixed in 80 mL of ethanol, and the solution refluxed for 16 hours. The reaction mixture was concentrated to 50 mL by removal of solvent under reduced pressure, and 20 mL of water was added. The remaining mixture was acidified to pH 5 with acetic acid, affording a white precipitate. The precipitate was collected by filtration, washed with water, and dried in a vacuum oven to give 2-amino-4-hydroxy-6-tert-butylpyrimidine (12.6 g), m.p. 285-288° C. (dec.).

後処理

  1. temperaturethe solution refluxed for 16 hours
  2. concentrationThe reaction mixture was concentrated to 50 mL by removal of solvent under reduced pressure, and 20 mL of water
  3. additionwas added
  4. customaffording a white precipitate
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water
  7. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-3935bcc626be4458859a6021f564f99f
出典データセット
uspto-grants-1999_09
特許番号
US05952331

関連ノート

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