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

HRID 27058

反応式

HRID 27058 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e92d68471f384dd693101c367d0b9ebe
出典データセット
uspto-grants-1980_09
特許番号
US04220603

関連ノート

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