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Diisopropylethylamine → 4-(4'-Chloro-biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acid

HRID 2266795
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2266795
C1C=CC(C(Cl)([C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][CH:15]=2)C2C=CC=CC=2)=CC=1.I[C:23]1[CH:39]=[CH:38][C:26]([O:27][CH2:28][C:29]2[CH:30]=[C:31]([C:35]([OH:37])=[O:36])[O:32][C:33]=2[CH3:34])=[CH:25][CH:24]=1.C(N(C(C)C)CC)(C)C>ClCCl>[Cl:20][C:19]1[CH:14]=[CH:15][C:16]([C:23]2[CH:39]=[CH:38][C:26]([O:27][CH2:28][C:29]3[CH:30]=[C:31]([C:35]([OH:37])=[O:36])[O:32][C:33]=3[CH3:34])=[CH:25][CH:24]=2)=[CH:17][CH:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 945242-Chlorotrityl chlorideHCID 184446544-(4-Iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid

Produkt 1

HCID 184445594-(4'-Chloro-biphenyl-4-yloxymethyl)-5-methyl-furan-2-carboxylic acidAusbeute 3,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344Dichloromethane
Lösungsmittel
2×

Versuchsvorschrift

2-Chlorotrityl chloride resin (2.55 g of nominal loading 1.3 mmol/g) was swelled with dichloromethane (20 mL). After draining, a solution of 4-(4-iodo-phenoxymethyl)-5-methyl-furan-2-carboxylic acid (26) (1.18 g) and diisopropylethylamine (2.3 mL) in dichloromethane (30 mL) was added and the mixture was shaken at room temperature for 72 hours. The resin was drained, washed sequentially with dichloromethane/triethylamine/methanol (20:1:3 by volume) (3×30 mL), dichloromethane (6×30 mL), N,N-dimethylformamide (2×25 mL), dichloromethane (6×25 mL), and diethyl ether (2×25 mL) and dried at 40° C. in vacuo, (ii) A stirred mixture of the resin from (i) (0.38 g), 4-chlorophenylboronic acid (0.30 g), [1,1′-bis-(diphenylphosphino)-ferrocene]-dichloropalladium(II) complex with dichloromethane (1:1) (30 mg), potassium acetate (0.20 g) in N,N-dimethylformamide (15 mL) was heated at 40° C. for 48 hours. The resin was drained, then washed sequentially with tetrahydrofuran/water (1:1 by volume), tetrahydrofuran, N,N-dimethylformamide, dichloromethane, diethyl ether and then dried at 45° C. in vacuo. The resin was treated with dichloromethane/trifluoroacetic acid (19:1 by volume) (20 mL) for 20 mins and the solution drained from the resin. This procedure was repeated. The combined solutions were concentrated in vacuo and the residue purified by HPLC to afford compound 27 as a white solid (43 mg). LC/MS System D: Rt=8.83 mins, m/z (ES−)=341 (M− for C19H15ClO4).

Aufarbeitung

  1. washwashed sequentially with dichloromethane/triethylamine/methanol (20:1:3 by volume) (3×30 mL), dichloromethane (6×30 mL), N,N-dimethylformamide (2×25 mL), dichloromethane (6×25 mL), and diethyl ether (2×25 mL)
  2. dry with materialdried at 40° C. in vacuo, (ii)
  3. additionA stirred mixture of the resin from (i) (0.38 g), 4-chlorophenylboronic acid (0.30 g), [1,1′-bis-(diphenylphosphino)-ferrocene]-dichloropalladium(II) complex with dichloromethane (1:1) (30 mg), potassium acetate (0.20 g) in N,N-dimethylformamide (15 mL)
  4. temperaturewas heated at 40° C. for 48 hours
  5. washwashed sequentially with tetrahydrofuran/water (1:1 by volume), tetrahydrofuran, N,N-dimethylformamide, dichloromethane, diethyl ether
  6. customdried at 45° C. in vacuo
  7. additionThe resin was treated with dichloromethane/trifluoroacetic acid (19:1 by volume) (20 mL) for 20 mins
  8. concentrationThe combined solutions were concentrated in vacuo
  9. customthe residue purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-0893c2e08b3b4dddb1cf68c452717102
Quelldatensatz
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07858644B2

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