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

Ammonium Acetate → 5-(2-Aminopropyl)benzofuran

HRID 1824943
ノート
印刷プレビュー

反応式

HRID 1824943 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][C:11](=O)[CH3:12])=[CH:9][C:4]=2[CH:3]=[CH:2]1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:20].[Na+]>CO>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]([NH2:20])[CH3:12])=[CH:9][C:4]=2[CH:3]=[CH:2]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 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 221447181-(1-benzofuran-5-yl)propan-2-one

生成物 1

HCID 98372325-(2-Aminopropyl)benzofuran収率 49.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 1 gm (5.7 mMol) 1-(benzofur-5-yl)-2-propanone, 8.9 gm (115 mMol) ammonium acetate, and 2.8 gm powdered 3A molecular sieves in 60 mL methanol was stirred at room temperature for 1 hour. To this mixture were then added 5.8 mL (5.8 mMol) sodium cyanoborohydride (1.0 M in tetrahydrofuran) and the mixture was stirred for an additional 5 hours at room temperature under a nitrogen atmosphere. The reaction mixture was then filtered over a pad of celite and the pad was rinsed with 200 mL methanol and 200 mL dichloromethane. The combined filtrates were concentrated under reduced pressure and the resultant residue was partitioned between 200 mL dichloromethane and 20 mL water. The mixture was washed with two 25 mL portions of 5 N sodium hydroxide. The combined aqueous extracts were extracted with three 100 mL portions of dichloromethane. All of the organic phases were combined, washed with 25 mL 0.1 N sodium hydroxide followed by 25 mL water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with a gradient of dichloromethane containing 6% methanol to dichloromethane containing 9% methanol and 9% concentrated ammonium hydroxide. Fractions containing product were combined and concentrated under reduced pressure to provide 0.498 gm (49%) of 1-(benzofur-5-yl)-2-aminopropane.

後処理

  1. stirringthe mixture was stirred for an additional 5 hours at room temperature under a nitrogen atmosphere
  2. filtrationThe reaction mixture was then filtered over a pad of celite
  3. washthe pad was rinsed with 200 mL methanol and 200 mL dichloromethane
  4. concentrationThe combined filtrates were concentrated under reduced pressure
  5. customthe resultant residue was partitioned between 200 mL dichloromethane and 20 mL water
  6. washThe mixture was washed with two 25 mL portions of 5 N sodium hydroxide
  7. extractionThe combined aqueous extracts were extracted with three 100 mL portions of dichloromethane
  8. washwashed with 25 mL 0.1 N sodium hydroxide
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. washeluting with a gradient of dichloromethane containing 6% methanol to dichloromethane containing 9% methanol and 9% concentrated ammonium hydroxide
  12. additionFractions containing product
  13. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-69a240273adf470288ccfbeee0faf990
出典データセット
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07045545B1

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