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

HRID 52187

반응식

HRID 52187 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c48b2d98f97457b9551f2e75bdadaf4
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616596

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