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Hydrochloric Acid → HCID 59016024、化合物

HRID 968829
ノート
印刷プレビュー

反応式

HRID 968829 の反応式
[O-]CC.[Na+].C(OCC)(=O)C.[OH:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH2:20][C:21]2[N:22]([CH2:35][CH2:36][CH3:37])[C:23](=[O:34])[N:24]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][CH:28]=3)[N:25]=2)=[CH:14][CH:13]=1.[C:38]([O:43][CH:44](CC)[CH2:45]CC)(=[O:42])[CH:39]([CH3:41])[CH3:40].Cl>C(O)C.O.C(OC(CC)CCC)(=O)C(C)C>[CH2:44]([O:43][C:38](=[O:42])[C:39]([CH3:41])([O:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH2:20][C:21]2[N:22]([CH2:35][CH2:36][CH3:37])[C:23](=[O:34])[N:24]([CH2:26][C:27]3[CH:28]=[CH:29][C:30]([CH3:33])=[CH:31][CH:32]=3)[N:25]=2)=[CH:14][CH:13]=1)[CH3:40])[CH3:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 2723922Sodium ethoxide5 回HCID 58579265Ethyl-2-butyl isobutyrate3 回HCID 59015891HCID 59015891、化合物

生成物 1

HCID 59016024HCID 59016024、化合物収率 63%

試薬・触媒・溶媒 3

HCID 58579265Ethyl-2-butyl isobutyrate触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a mixture of sodium ethoxide (1.22 mL, 3.28 mmol) and ethyl acetate (322 μL, 3.28 mmol) was added 5-[3-(4-hydroxyphenyl)-propyl]-2-(4-methylbenzyl)-4-propyl-2,4-dihydro-[1,2,4]triazol-3-one (1.2 g, 3.28 mmol) in ethanol (10 mL) and the resulting mixture stirred at reflux for 1 hour. Then ethyl-2-butyl isobutyrate (1.08 mL, 7.38 mmol) was added and the reaction continued at reflux for 1 hour. Then sodium ethoxide (1.22 mL, 3.28 mmol) was added dropwise over 5 min and the reaction continued at reflux for 4.5 hour. Additional sodium ethoxide (520 μL, 1.4 mmol) and ethyl-2-butyl isobutyrate (205 μL, 1.4 mmol) were added and reaction continued at reflux for 4 hour. Additional sodium ethoxide (336 μL, 0.903 mmol) and ethyl-2-butyl isobutyrate (132 μL, 0.903 mmol) were added and the reaction continued at reflux for 3 hours. Finally, additional sodium ethoxide (200 μL, 0.54 mmol) and ethyl-2-butyl isobutyrate (100 μL, 0.133 mmol) were added and the reaction continued at reflux for 1.5 hours. The mixture was allowed to cool to room temperature and is then quenched into a solution of conc. HCl (1.5 g, 41 mmol) in water (50 mL). The resulting solution was then concentrated in vacuo, taken up in ethyl acetate (100 mL) and the aqueous layer was discarded. The organic layer was washed with saturated aq. NaHCO3 (2×50 mL) followed by saturated aq. NaCl (2×25 mL). The organic layer was dried (MgSO4), filtered, concentrated, and purified by silica gel chromatography (1:1 ethyl acetate:hexanes) to afford the title compound as a yellow oil (990 mg, 2.06 mmol, 63%):

後処理

  1. temperatureat reflux for 1 hour
  2. temperatureat reflux for 1 hour
  3. temperatureat reflux for 4.5 hour
  4. customreaction
  5. temperatureat reflux for 4 hour
  6. temperatureat reflux for 3 hours
  7. temperatureat reflux for 1.5 hours
  8. concentrationThe resulting solution was then concentrated in vacuo
  9. washThe organic layer was washed with saturated aq. NaHCO3 (2×50 mL)
  10. dry with materialThe organic layer was dried (MgSO4)
  11. filtrationfiltered
  12. concentrationconcentrated
  13. custompurified by silica gel chromatography (1:1 ethyl acetate:hexanes)

出典と根拠

ORDレコード
ord-678a312068fe442b9c7941984493004d
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07304062B2

反応ノート

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