Triethylamine → Ethyl 1,4-dibenzylpiperazine-2-carboxylate

HRID 248452

反応式

HRID 248452 の反応式
Br[CH:2]([CH2:8]Br)[C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH2:10]([NH:17][CH2:18][CH2:19][NH:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:22]1([CH2:21][N:20]2[CH2:19][CH2:18][N:17]([CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:8][CH:2]2[C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 8793BenzathineHCID 97945Ethyl 2,3-dibromopropionate

生成物 1

HCID 2736402Ethyl 1,4-dibenzylpiperazine-2-carboxylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
80 °C

実験手順

A 29.1 g portion of 2,3-dibromopropionic acid, ethyl ester was dissolved in 90 ml of dry toluene at 40° C. in an oil bath. With vigorous stirring, a stream of a solution of 26.8 g of N,N'-dibenzylethylenediamine and 30.5 ml of triethylamine in 28 ml of dry toluene was added. The temperature was raised to 80° C. and stirring continued for 3 hours. The mixture was filtered, the solid washed with two 50 ml portions of toluene and the filtrate and washes combined. The solution was washed with three 50 ml portions of water, dried, filtered and concentrated to an oil. The oil was distilled and the fraction boiling at 185°-195° C., 0.75 mm collected, giving 1,4-bis(phenylmethyl)-2-piperazinecarboxylic acid, ethyl ester as a yellow oil.

後処理

  1. filtrationThe mixture was filtered
  2. washthe solid washed with two 50 ml portions of toluene
  3. washThe solution was washed with three 50 ml portions of water
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated to an oil
  7. distillationThe oil was distilled
  8. customthe fraction boiling at 185°-195° C., 0.75 mm collected

出典と根拠

ORDレコード
ord-46a2058602874a9c8ed59da2773d4f6b
出典データセット
uspto-grants-1993_05
特許番号
US05210193

関連ノート

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