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Cyclopropanecarboximidamide hydrochloride → 2-Cyclopropylpyrimidin-4-ol

HRID 386109
ノート
印刷プレビュー

反応式

HRID 386109 の反応式
C(O[C:4](=[O:8])/[CH:5]=[CH:6]\[O-])C.[Na+].Cl.[CH:11]1([C:14](=[NH:16])[NH2:15])[CH2:13][CH2:12]1>O>[CH:11]1([C:14]2[N:16]=[C:4]([OH:8])[CH:5]=[CH:6][N:15]=2)[CH2:13][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2781916Cyclopropanecarboximidamide hydrochlorideHCID 58190618sodium (Z)-3-ethoxy-3-oxoprop-1-en-1-olate

生成物 1

HCID 1785164792-Cyclopropylpyrimidin-4-ol

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Sodium (1Z)-3-ethoxy-3-oxoprop-1-en-1-olate (6.60 g, 47.8 mmol) was dissolved in water (1.5 mL) and in a second flask cyclopropanecarboximidamide hydrochloride (3 g, 24.88 mmol) was dissolved in water (2 mL) and the contents of the second flask were added to the first flask. The reaction was allowed to stir for 72 hours. The reaction was then transferred to a separatory funnel and extracted with chloroform and a small amount of methanol. The water layer was extracted again and the combined organic layers were dried over magnesium sulfate, filtered and concentrated to a pale yellow solid. Diethyl ether was then added to precipitate product. The mixture was filtered and the solid was collected and dried to give the title compound.

後処理

  1. additionthe contents of the second flask were added to the first flask
  2. customThe reaction was then transferred to a separatory funnel
  3. extractionextracted with chloroform
  4. extractionThe water layer was extracted again
  5. dry with materialthe combined organic layers were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to a pale yellow solid
  8. additionDiethyl ether was then added
  9. customto precipitate product
  10. filtrationThe mixture was filtered
  11. customthe solid was collected
  12. customdried

出典と根拠

ORDレコード
ord-708040ad3ea242c584d8d16a9ff0b2e5
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367706B2

反応ノート

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