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1,1-Dichloroethane → (S)-tert-butyl 2-(6-(7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzo[b,d]thiophen-3-yl)-1H-benzo[d]imidazol-2-yl)pyrrolidine-1-carboxylate

HRID 1751377
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1751377
CC1(C)C(C)(C)OB([C:9]2[CH:10]=[CH:11][C:12]3[C:16]4[CH:17]=[CH:18][C:19]([B:21]5[O:25][C:24]([CH3:27])([CH3:26])[C:23]([CH3:29])([CH3:28])[O:22]5)=[CH:20][C:15]=4[S:14][C:13]=3[CH:30]=2)O1.Br[C:33]1[CH:34]=[CH:35][C:36]2[N:40]=[C:39]([C@@H:41]3[CH2:45][CH2:44][CH2:43][N:42]3[C:46]([O:48][C:49]([CH3:52])([CH3:51])[CH3:50])=[O:47])[NH:38][C:37]=2[CH:53]=1.C(=O)([O-])[O-].[K+].[K+].ClC(Cl)C>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1(C)C=CC=CC=1.C(COC)OC>[CH3:27][C:24]1([CH3:26])[C:23]([CH3:28])([CH3:29])[O:22][B:21]([C:19]2[CH:18]=[CH:17][C:16]3[C:12]4[CH:11]=[CH:10][C:9]([C:33]5[CH:34]=[CH:35][C:36]6[N:40]=[C:39]([C@@H:41]7[CH2:45][CH2:44][CH2:43][N:42]7[C:46]([O:48][C:49]([CH3:51])([CH3:50])[CH3:52])=[O:47])[NH:38][C:37]=6[CH:53]=5)=[CH:30][C:13]=4[S:14][C:15]=3[CH:20]=2)[O:25]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 63651,1-DichloroethaneHCID 11430Potassium CarbonateHCID 56605032(S)-tert-butyl 2-(6-bromo-1H-benzo[d]imidazol-2-yl)pyrrolidine-1-carboxylateHCID 676817643,7-Bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzothiophene

Produkt 1

HCID 67681976
(S)-tert-butyl 2-(6-(7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzo[b,d]thiophen-3-yl)-1H-benzo[d]imidazol-2-yl)pyrrolidine-1-carboxylate
Ausbeute 62,2 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 1140TolueneLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A mixture of 3,7-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-dibenzo[b,d]thiophene (3.6 g, 8.2 mmol), (S)-tert-butyl 2-(6-bromo-1H-benzo[d]imidazol-2-yl)pyrrolidine-1-carboxylate (1.0 g, 2.7 mmol), tetrakis(triphenylphosphine)palladium(0) (0.31 mg, 0.27 mmol), 2M aqueous potassium carbonate solution (5 mL, 10 mmol), dimethoxyethane (25 mL), toluene (5 mL) and dichloroethane (2.5 mL) was degassed under a stream of argon for 15 minutes. The reaction was heated to 85° C. for 2 hours. Upon completion, the reaction was cooled to room temperature, diluted with ethyl acetate and filtered through Celite. The filtrate was washed with water and brine, dried (MgSO4) and concentrated. The resulting crude material was purified by flash column chromatography to yield (S)-tert-butyl 2-(6-(7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzo[b,d]thiophen-3-yl)-1H-benzo[d]imidazol-2-yl)pyrrolidine-1-carboxylate (1.0 g, 62%).

Aufarbeitung

  1. customwas degassed under a stream of argon for 15 minutes
  2. temperatureUpon completion, the reaction was cooled to room temperature
  3. additiondiluted with ethyl acetate
  4. filtrationfiltered through Celite
  5. washThe filtrate was washed with water and brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customThe resulting crude material was purified by flash column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-933b68e1cd6e41858449711bde398393
Quelldatensatz
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09156823B2

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