Diisopropylethylamine → 2-[4-(5-Bromo-2-methoxybenzyl)-1-piperazinyl]pyrimidine

HRID 234116

反応式

HRID 234116 の反応式
Cl[CH2:2][C:3]1[CH:8]=[C:7]([Br:9])[CH:6]=[CH:5][C:4]=1[O:10][CH3:11].Cl.Cl.[N:14]1[CH:19]=[CH:18][CH:17]=[N:16][C:15]=1[N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.C(N(CC)C(C)C)(C)C>C(Cl)(Cl)Cl>[N:14]1[CH:19]=[CH:18][CH:17]=[N:16][C:15]=1[N:20]1[CH2:25][CH2:24][N:23]([CH2:2][C:3]2[CH:8]=[C:7]([Br:9])[CH:6]=[CH:5][C:4]=2[O:10][CH3:11])[CH2:22][CH2:21]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 103540684-Bromo-2-(chloromethyl)-1-methoxybenzeneHCID 116802722-Piperazinylpyrimidine dihydrochloride

生成物 1

HCID 12403032-[4-(5-Bromo-2-methoxybenzyl)-1-piperazinyl]pyrimidine収率 235%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 1.1 g of 2-(chloromethyl)-4-bromoanisole, 1 g of 1-(2-pyrimidyl)piperazine dihydrochloride and 2.0 mL N,N-diisopropylethylamine in 10 mL chloroform was heated at reflux temperature for 2 hr, cooled to room temperature, washed with 1N NaOH and water. The solvent was removed by evaporation under reduced pressure to yield 3.6 g of 2-[(4-(2-pyrimidinyl)-piperazinyl)methyl]-4-bromoanisole as a white solid which was used in the next step without further purification.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 2 hr
  3. washwashed with 1N NaOH and water
  4. customThe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-50c7e7e5bd1142ff86cca652ef994649
出典データセット
uspto-grants-1997_01
特許番号
US05594141

関連ノート

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