Triethylamine → Methyl 4-[(4-diphenylmethyl-1-piperazinyl)methyl]phenylacetate

HRID 481297

反応式

HRID 481297 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:5][CH:4]=1.[CH:14]([N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C>O1CCOCC1>[C:21]1([CH:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:27]2[CH2:28][CH2:29][N:30]([CH2:2][C:3]3[CH:8]=[CH:7][C:6]([CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:5][CH:4]=3)[CH2:31][CH2:32]2)[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 70048BenzhydrylpiperazineHCID 11770640Methyl 2-(4-(bromomethyl)phenyl)acetate

生成物 1

HCID 10993378Methyl 4-[(4-diphenylmethyl-1-piperazinyl)methyl]phenylacetate収率 90.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A 200 ml eggplant-shaped flask was charged with 5.38 g of methyl 4-bromomethylphenylacetate, 6.06 g of 1-benzhydrylpiperazine, 6.1 ml of triethylamine, and 100 ml of dioxane and the mixture was stirred at room temperature for 5 hours. The solvent was then distilled off and the residue was extracted with ethyl acetate. The extract was washed with water, the solvent was distilled off, and the residue was recrystallized from methanol to provide 8.33 g of methyl 4-[(4-diphenylmethyl-1-piperazinyl)methyl]phenylacetate melting at 124° C.-125° C.

後処理

  1. distillationThe solvent was then distilled off
  2. extractionthe residue was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. distillationthe solvent was distilled off
  5. customthe residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-89b68ced720c466195934876f641ea89
出典データセット
uspto-grants-1998_08
特許番号
US05789409

関連ノート

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