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Cyclopropyl methyl ketone → 1-Cyclopropyl-3-(3-pyridazinyl)-1,3-propanedione

HRID 1076689
ノート
印刷プレビュー

反応式

HRID 1076689 の反応式
C(O[C:4]([C:6]1[N:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5])C.[CH:12]1([C:15]([CH3:17])=[O:16])[CH2:14][CH2:13]1.C[O-].[Na+]>C1C=CC=CC=1>[CH:12]1([C:15](=[O:16])[CH2:17][C:4]([C:6]2[N:7]=[N:8][CH:9]=[CH:10][CH:11]=2)=[O:5])[CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 13004Cyclopropyl methyl ketoneHCID 10942334Sodium MethoxideHCID 14452007Ethyl pyridazine-3-carboxylate

生成物 1

HCID 123605611-Cyclopropyl-3-(3-pyridazinyl)-1,3-propanedione

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A stirred mixture of 4.0 g. of ethyl-3-pyridazinecarboxylate, 4.4 g. of cyclopropylmethyl ketone and 1.6 g. of sodium methoxide in 100 ml. of benzene is heated under reflux for 5 hours. The mixture is diluted with 300 ml. of water and the benzene phase is separated. The aqueous mixture is made weakly acidic with dilute hydrochloric acid and extracted with chloroform. The chloroform solution is dried over magnesium sulfate and concentrated under reduced pressure to yield straw-colored crystals which are recrystallized from acetonitrile to give cream-colored crystals, melting point 85°-87°C.

後処理

  1. additionA stirred mixture of 4.0 g
  2. temperatureunder reflux for 5 hours
  3. additionThe mixture is diluted with 300 ml
  4. customof water and the benzene phase is separated
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform solution is dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto yield straw-colored crystals which
  9. customare recrystallized from acetonitrile
  10. customto give cream-colored crystals, melting point 85°-87°C.

出典と根拠

ORDレコード
ord-dee5d170abcf4ec79a490c1160d16b96
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03957805

反応ノート

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