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2-Methyl-2-butene → 5-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carboxylic acid

HRID 1054658
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1054658
[OH:1][C:2]1([C:6]2[CH:11]=[CH:10][C:9]([C:12]3[CH:13]=[C:14]4[C:18](=[CH:19][C:20]=3[CH3:21])[NH:17][CH:16]=[C:15]4[CH:22]=[O:23])=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3]1.CC(=CC)C.Cl([O-])=[O:30].[Na+].O.OP([O-])(O)=O.[Na+].[Cl-].[NH4+]>O1CCCC1.C(O)(C)(C)C.O>[OH:1][C:2]1([C:6]2[CH:11]=[CH:10][C:9]([C:12]3[CH:13]=[C:14]4[C:18](=[CH:19][C:20]=3[CH3:21])[NH:17][CH:16]=[C:15]4[C:22]([OH:30])=[O:23])=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3]1
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Komponenten

9

Edukt 5

HCID 105532-Methyl-2-buteneHCID 25517Ammonium ChlorideHCID 516949Sodium Phosphate, Monobasic, MonohydrateHCID 23668197Sodium ChloriteHCID 866986615-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carbaldehyde

Produkt 1

HCID 86698662
5-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6386tert-ButanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A partial suspension of 5-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carbaldehyde (130 mg, 0.426 mmol) in tetrahydrofuran (3 mL) and tert-butanol (3 mL) was treated with 2-methyl-2-butene (2.27 mL, 21.4 mmol) followed by a solution of sodium chlorite (538 mg, 6.4 mmol) and sodium phosphate monobasic hydrate (904 mg, 6.5 mmol) in water (2 mL) via glass pipet at room temperature. The reaction mixture was stirred vigorously at room temperature for 62 hours, and was poured into half-diluted saturated aqueous ammonium chloride solution (50 mL). The product was extracted with ethyl acetate (3×60 mL), and the combined organic layers were dried over sodium sulfate, filtered and evaporated. The crude product was purified using reverse-phase chromatography to give the title compound.

Aufarbeitung

  1. extractionThe product was extracted with ethyl acetate (3×60 mL)
  2. dry with materialthe combined organic layers were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude product was purified

Quellen und Nachweise

ORD-Eintrag
ord-10dc6b922c2c4b17b9229c5202338e88
Quelldatensatz
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09394285B2

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