Acetic Anhydride → N-(6-aminopyrimidin-4-yl)acetamide

HRID 2366202

反応式

HRID 2366202 の反応式
[N:1]1[C:6]([NH2:7])=[CH:5][C:4]([NH2:8])=[N:3][CH:2]=1.[C:9](OC(=O)C)(=[O:11])[CH3:10]>O1CCOCC1>[NH2:8][C:4]1[N:3]=[CH:2][N:1]=[C:6]([NH:7][C:9](=[O:11])[CH3:10])[CH:5]=1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 79608Pyrimidine-4,6-diamine

生成物 1

HCID 3031498N-(6-aminopyrimidin-4-yl)acetamide収率 61%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a stirred suspension of pyrimidine-4,6-diamine (500 mg, 4.55 mmol) in dioxane (20 mL) was added acetic anhydride (465 mg, 4.55 mmol) and the resulting mixture was heated under reflux for 15 hours. The reaction was cooled to room temperature and the resulting precipitate was collected by filtration. The filtercake was dissolved in 1N HCl and the pH of the aqueous phase adjusted to 7 by the addition of 1N NaOH. The resulting white precipitate was collected by filtration and dried to afford the desired product as a white solid (420 mg, 61% yield). LCMS (ESI) m/z: 152.0 [M+H+].

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 15 hours
  3. filtrationthe resulting precipitate was collected by filtration
  4. dissolutionThe filtercake was dissolved in 1N HCl
  5. additionthe pH of the aqueous phase adjusted to 7 by the addition of 1N NaOH
  6. filtrationThe resulting white precipitate was collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-df25aac569e74280ab2451790da6bd3b
出典データセット
uspto-grants-2014_04
特許番号
US08697708B2

関連ノート

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