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Hydrochloric Acid → 3-({[4-(Cyclohexyl{2-ethyl-5-[4-(trifluoromethyl)phenyl]thiophen-3-yl}methoxy)phenyl]carbonyl}amino)propanoic acid

HRID 1876992
ノート
印刷プレビュー

反応式

HRID 1876992 の反応式
C1([CH:7]([C:18]2[CH:22]=[C:21]([C:23]3[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=3)[S:20][C:19]=2[CH2:33][CH3:34])[O:8][C:9]2[CH:17]=[CH:16][C:12]([C:13](O)=[O:14])=[CH:11][CH:10]=2)CCCCC1.Cl.[NH2:36][CH2:37][CH2:38][C:39]([O:41]CC)=[O:40].O.ON1[C:50]2[CH:51]=[CH:52][CH:53]=[CH:54][C:49]=2N=N1.Cl.C(N=C=NCCCN(C)C)C.[Cl-].[NH4+].[OH-].[Na+].Cl>C(O)C.O1CCCC1.CN(C)C=O.C(N(CC)CC)C>[CH:49]1([CH:7]([C:18]2[CH:22]=[C:21]([C:23]3[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:30])[F:31])=[CH:25][CH:24]=3)[S:20][C:19]=2[CH2:33][CH3:34])[O:8][C:9]2[CH:10]=[CH:11][C:12]([C:13]([NH:36][CH2:37][CH2:38][C:39]([OH:41])=[O:40])=[O:14])=[CH:16][CH:17]=2)[CH2:54][CH2:53][CH2:52][CH2:51][CH2:50]1
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 7

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrate
HCID 68514596
4-(Cyclohexyl{2-ethyl-5-[4-(trifluoromethyl)phenyl]thiophen-3-yl}methoxy)benzoic acid

生成物 1

HCID 595294123-({[4-(Cyclohexyl{2-ethyl-5-[4-(trifluoromethyl)phenyl]thiophen-3-yl}methoxy)phenyl]carbonyl}amino)propanoic acid収率 40.7%

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

To a mixture of 4-(cyclohexyl{2-ethyl-5-[4-(trifluoromethyl)phenyl]thiophen-3-yl}methoxy)benzoic acid (251 mg) synthesized above, ethyl β-alaninate hydrochloride (94.8 mg), 1-hydroxybenzotriazole monohydrate (94.5 mg), triethylamine (86.0 μL) and N,N-dimethylformamide (10 mL) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (118 mg), and the mixture was stirred at room temperature for 3 hr. Saturated aqueous ammonium chloride solution was added to quench the reaction, and the mixture was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane to ethyl acetate:hexane=2:3, volume ratio) to give a colorless oil. To a mixture of the obtained oil, tetrahydrofuran (5 mL) and ethanol (5 mL) was added 1N aqueous sodium hydroxide solution (2 mL), and the mixture was stirred at room temperature for 1 hr. 1N Hydrochloric acid (2.5 mL) was added to the reaction mixture, the organic solvent was evaporated under reduced pressure, and the mixture was extracted with ethyl acetate. The extract was washed with water and brine, dried over magnesium sulfate and concentrated under reduced pressure to give a white solid. The solid was recrystallized from ethyl acetate-hexane to give the title compound (117 mg, 40%) as a colorless crystal.

後処理

  1. customto quench
  2. customthe reaction
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane to ethyl acetate:hexane=2:3, volume ratio)
  8. customto give a colorless oil
  9. stirringthe mixture was stirred at room temperature for 1 hr
  10. customthe organic solvent was evaporated under reduced pressure
  11. extractionthe mixture was extracted with ethyl acetate
  12. washThe extract was washed with water and brine
  13. dry with materialdried over magnesium sulfate
  14. concentrationconcentrated under reduced pressure
  15. customto give a white solid
  16. customThe solid was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-d96e0378ce254e98a17a3cff64e325cd
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309580B2

反応ノート

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