N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine → 1H-Indene-3-ethanamine

HRID 1534797ノート

反応式

HRID 1534797 の反応式
[CH:1]1([CH2:10][CH2:11][NH:12]O)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1>C(O)(=O)C.[Zn]>[CH2:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[C:1]([CH2:10][CH2:11][NH2:12])=[CH:2]1

参加物

4

反応物 1

HCID 19908298N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine

生成物 1

HCID 5339401H-Indene-3-ethanamine

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine (85 mg, 0.486 mmol) was added to a slurry of zinc dust (104 mg, 1.59 mmol) in glacial acetic acid (3 ml), and the mixture was heated at 65° for 2 hours. The mixture was cooled and filtered, then made basic with conc. ammonium hydroxide and extracted with ether. The ether layer was washed with water, then with brine, dried ober sodium sulfate, filtered, and evaporated to dryness in vacuo. The residue was chromatographed on a silica gel column eluted with 90:10:1 of CH2Cl2 :MeOH:NH4OH. The product fractions were evaporated to dryness in vacuo to give (2-(1H-indene-3-yl)ethyl)amine.

後処理

  1. temperaturethe mixture was heated at 65° for 2 hours
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. extractionextracted with ether
  5. washThe ether layer was washed with water
  6. dry with materialwith brine, dried ober sodium sulfate
  7. filtrationfiltered
  8. customevaporated to dryness in vacuo
  9. customThe residue was chromatographed on a silica gel column
  10. washeluted with 90:10:1 of CH2Cl2
  11. customThe product fractions were evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-d4d669521c0642a4a1a8a890b93ac5cd
出典データセット
uspto-grants-1992_02
特許番号
US05091387

反応ノート

読み込み中…