Tetrahydrofuran → 3-[4-(3,3-Diphenyl-1-propyl)piperazin-1-yl]benzoic acid

HRID 1796736ノート

反応式

HRID 1796736 の反応式
[C:1]1([CH:7]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:17]=[C:18]([CH:24]=[CH:25][CH:26]=3)[C:19]([O:21]CC)=[O:20])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O1CCCC1.[OH-].[Na+]>CO>[C:27]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([C:16]3[CH:17]=[C:18]([CH:24]=[CH:25][CH:26]=3)[C:19]([OH:21])=[O:20])[CH2:14][CH2:15]2)[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 22180549Ethyl 3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]benzoate

生成物 1

HCID 221804873-[4-(3,3-Diphenyl-1-propyl)piperazin-1-yl]benzoic acid収率 85.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

The compound (2.00 g) prepared in step (b) was dissolved in a mixed solvent composed of tetrahydrofuran (20 ml) and methanol (10 ml), and a 1 mol/l aqueous sodium hydroxide solution (10 ml) was added to the solution. The mixture was then stirred at 65° C. for one hr. The solvent was removed from the reaction solution by distillation under the reduced pressure. Water (30 ml) was then added to the residue, and the mixture was adjusted to pH 4 by the addition of 1 mol/l hydrochloric acid. The resultant precipitate was collected by filtration, and was then dried to give 1.60 g (85.6%) of 3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]benzoic acid.

後処理

  1. customThe solvent was removed from the reaction solution by distillation under the reduced pressure
  2. additionWater (30 ml) was then added to the residue
  3. additionthe mixture was adjusted to pH 4 by the addition of 1 mol/l hydrochloric acid
  4. filtrationThe resultant precipitate was collected by filtration
  5. customwas then dried

出典と根拠

ORDレコード
ord-5ad28e1e4c184bc4a7fbe526ccc40118
出典データセット
uspto-grants-2006_04
特許番号
US07030120B2

反応ノート

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