4-Piperidinecarboxamide → 2-[2-(4-Carbamoylpiperidino)ethoxy]bibenzyl

HRID 27058

반응식

HRID 27058 반응식
Br[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[NH:19]1[CH2:24][CH2:23][CH:22]([C:25]([NH2:27])=[O:26])[CH2:21][CH2:20]1>O1CCCC1.O>[C:25]([CH:22]1[CH2:23][CH2:24][N:19]([CH2:2][CH2:3][O:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:20][CH2:21]1)(=[O:26])[NH2:27]

참가 물질

5

반응물 2

HCID 37724-PiperidinecarboxamideHCID 205450162-(2-Bromoethoxy)bibenzyl

생성물 1

HCID 128525822-[2-(4-Carbamoylpiperidino)ethoxy]bibenzyl수율 82.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2 g of 2-(2-bromoethoxy)bibenzyl and 1.7 g of 4-piperidinecarboxamide in 20 ml of tetrahydrofuran and 10 ml of water was stirred at 70° C. for 10 hours. The reaction mixture was concentrated and to the residue was added 1 N NaOH aqueous solution. The resultant crystals were filtered, washed well with water and then recrystallized from ethanol to give 1.9 g (82% yield) of 2-[2-(4-carbamoylpiperidino)ethoxy]bibenzyl, m. p. 60°-63° C.

후처리

  1. concentrationThe reaction mixture was concentrated and to the residue
  2. additionwas added 1 N NaOH aqueous solution
  3. filtrationThe resultant crystals were filtered
  4. washwashed well with water
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-e92d68471f384dd693101c367d0b9ebe
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220603

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