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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Cyclopropylamine → HCID 13579376、化合物

HRID 1589081
ノート
印刷プレビュー

反応式

HRID 1589081 の反応式
[C:1]1([CH:7]2[C:11](=[O:12])[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=3)=[C:9]([NH2:23])[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:24]1(N)[CH2:26][CH2:25]1>C(O)C>[C:1]1([CH:7]2[C:11](=[O:12])[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:20])([F:21])[F:22])[CH:14]=3)=[C:9]([NH:23][CH:24]3[CH2:26][CH2:25]3)[O:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=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 69828Cyclopropylamine2 回HCID 13579285HCID 13579285、化合物

生成物 1

HCID 13579376HCID 13579376、化合物収率 36.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In this example, a mixture containing 5.0 g (0.0157 g mole) of 2-phenyl-3-oxo-4-(3-trifluoromethylphenyl)-5-amino-2,3-dihydrofuran and 8.96 g of cyclopropylamine in 50 ml of ethanol containing 5% water was refluxed for six days. At the end of this time, a sample of the reaction mixture was checked by thin layer chromatography and then an additional 8.96 g of cyclopropylamine was added. The mixture was refluxed for an additional 24 hours and then allowed to stand at room temperature over night. The mixture was then concentrated by evaporation under vacuum, affording a crude product oil. The crude product was chromatographed over silica gel eluting with 80:20 (V/V) petroleum ether and ethyl acetate. The product fractions were combined and evaporated in vacuo affording 2.07 g of the title compound Elemental Analysis Carbon calc.: 66.8%, found 67.4%; hydrogen calc.: 4.5%, found 4.7%; nitrogen calc.: 3.9%, found 4.6%; melting point 160°-164° C.

後処理

  1. temperaturewas refluxed for six days
  2. temperatureThe mixture was refluxed for an additional 24 hours
  3. waitto stand at room temperature over night
  4. concentrationThe mixture was then concentrated by evaporation under vacuum
  5. customaffording a crude product oil
  6. customThe crude product was chromatographed over silica gel eluting with 80:20 (V/V) petroleum ether and ethyl acetate
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-36a69d75279c47b39577b0c812143b03
出典データセット
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04568378

反応ノート

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