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

Hydrazine hydrate (1:1) → 3,3,3-Trifluoro-1-(3-nitrophenyl)-1-propanone hydrazone

HRID 428969
ノート
印刷プレビュー

反応式

HRID 428969 の反応式
[F:1][C:2]([F:16])([F:15])[CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)=O.O.[NH2:18][NH2:19]>O1CCCC1>[F:1][C:2]([F:16])([F:15])[CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-:14])=[O:13])[CH:7]=1)=[N:18][NH2:19]
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 24654Hydrazine hydrate (1:1)HCID 221413423,3,3-Trifluoro-1-(3-nitrophenyl)-1-propanone

生成物 1

HCID 736985983,3,3-Trifluoro-1-(3-nitrophenyl)-1-propanone hydrazone収率 8.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3,3,3-Trifluoro-1-(3-nitrophenyl)-1-propanone (Sov. Prog. Chem. (Engl.Transi.), 1966, 32, 745, 1.8 g, 7.72 mmol) was dissolved in tetrahydrofuran (10 ml) and hydrazine monohydrate (0.56 ml, 11.58 mmol) was added dropwise at room temperature. The reaction mixture was stirred for 1 h at room temperature then heated under reflux for 40 min. The reaction mixture was concentrated in vacui and the residue treated with water (10 ml) and extracted with dichloromethane (4×10 ml). The organic extracts were concentrated in vacuo and the residue was purified by chromatography on silica gel (100 g), eluting with diciforomethane: hexane (1:1 and then 2:1). The product was obtained as an amber gum (159 mg, 8%).

後処理

  1. temperaturethen heated
  2. temperatureunder reflux for 40 min
  3. concentrationThe reaction mixture was concentrated in vacui
  4. additionthe residue treated with water (10 ml)
  5. extractionextracted with dichloromethane (4×10 ml)
  6. concentrationThe organic extracts were concentrated in vacuo
  7. customthe residue was purified by chromatography on silica gel (100 g)
  8. washeluting with diciforomethane

出典と根拠

ORDレコード
ord-c53229ee727247eaacefae25216cfb7a
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06313312B1

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