ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Triethylamine → HCID 178469368、化合物

HRID 2401176
ノート
印刷プレビュー

反応式

HRID 2401176 の反応式
Cl.[CH:2]([NH2:4])=[NH:3].[C:5](OCC)(=[O:13])[C:6]#[C:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C(N(CC)CC)C>C(#N)C>[OH:13][C:5]1[N:4]=[CH:2][N:3]=[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[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

5

反応物 3

HCID 8471TriethylamineHCID 69803Diethyl acetylenedicarboxylateHCID 10313058Methanimidamide, hydrochloride (1:1)

生成物 1

HCID 178469368HCID 178469368、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Formamidine hydrochloride (2.0 g, 45.4 mmol) and diethyl 2-butynedioate (7.23 mL, 45.4 mmol) were added together in acetonitrile (85 mL) and the resulting mixture was treated dropwise with triethylamine (6.33 mL, 45.4 mmol). The resulting mixture was heated under reflux for 4 hours. The reaction mixture was allowed to cool to room temperature, further cooled in an ice bath and the resulting solid was collected by filtration and discarded. The filtrate was evaporated under reduced pressure and the residue purified by column chromatography (Biotage SP4) eluting with a gradient of 0-100% ethyl acetate and iso-hexane. Product containing fractions were combined and evaporated under reduced pressure to give the title compound as an off white solid (0.995 g);

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperaturefurther cooled in an ice bath
  4. filtrationthe resulting solid was collected by filtration
  5. customThe filtrate was evaporated under reduced pressure
  6. customthe residue purified by column chromatography (Biotage SP4)
  7. washeluting with a gradient of 0-100% ethyl acetate and iso-hexane
  8. additionProduct containing fractions
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-92a82815666640f9bd5a7d737fa74e15
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08796283B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート