(2-Thienylmethyl)amine → 2-(Pyrrolodin-2-one-1-ylmethyl)thiophene

HRID 52187

反応式

HRID 52187 の反応式
Br[CH2:2][CH2:3][CH2:4][C:5]([O:7]CC)=O.[S:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][NH2:16].C(N(CC)C(C)C)(C)C>C1C=CC=CC=1>[N:16]1([CH2:15][C:11]2[S:10][CH:14]=[CH:13][CH:12]=2)[CH2:2][CH2:3][CH2:4][C:5]1=[O:7]

参加物

5

反応物 3

HCID 34005(2-Thienylmethyl)amineHCID 76300Ethyl 4-bromobutyrateHCID 81531Diisopropylethylamine

生成物 1

HCID 675888032-(Pyrrolodin-2-one-1-ylmethyl)thiophene収率 47.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of ethyl 4-bromobutyrate (5.85 g, 30.0 mmol), 2-thiophenemethylamine (13.6 g, 120 mmol), and N,N-diisopropylethylamine (3.88 g, 30.0 mmol) in benzene (100 mL) was stirred under N2 at reflux for 2 hours. The reaction mixture was cooled to ambient temperature and filtered. The residue was concentrated in vacuo, dissolved in ether, and washed twice with 2N aqueous HCl, and once with brine, then dried over MgSO4, filtered, and concentrated in vacuo to give 2-(pyrrolodin-2-one-1-ylmethyl)thiophene (2.59 g) as an oil.

後処理

  1. temperatureat reflux for 2 hours
  2. filtrationfiltered
  3. concentrationThe residue was concentrated in vacuo
  4. dissolutiondissolved in ether
  5. washwashed twice with 2N aqueous HCl
  6. dry with materialonce with brine, then dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9c48b2d98f97457b9551f2e75bdadaf4
出典データセット
uspto-grants-1997_04
特許番号
US05616596

関連ノート

読み込み中…