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

HRID 1796736노트

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HRID 1796736 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ad28e1e4c184bc4a7fbe526ccc40118
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030120B2

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