Methanol → 9-Ethyl-3-isocyanatocarbazole

HRID 2413673

Reaktionsgleichung

Reaktionsgleichung von HRID 2413673
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH2:15][CH3:16])[C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.C(N(CC)CC)C.[CH3:24][OH:25].C1(N=C=NC2CCCCC2)CCCCC1>C(=S)=S>[CH2:15]([N:6]1[C:5]2[CH:4]=[CH:3][C:2]([N:1]=[C:24]=[O:25])=[CH:14][C:13]=2[C:12]2[C:7]1=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH3:16]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 8471TriethylamineHCID 85883-Amino-9-ethylcarbazoleHCID 10868Dicyclohexylcarbodiimide

Produkt 1

HCID 201550999-Ethyl-3-isocyanatocarbazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

38.6 g of 3-amino-9-ethylcarbazole and 27.9 ml of triethylamine were added to 300 ml of methanol, and, while cooling with ice, 15.2 g of carbon disulfide was added dropwise thereto. After conducting reaction at room temperature for 3 hours, 41.3 g of dicyclohexylcarbodiimide was added thereto, followed by reacting at room temperature for 4 hours. Crystals thus precipitated were collected by filtration, heat-refluxed in 500 ml of ethyl acetate, and cooled to precipitate and then filter off solids. The filtrate was concentrated to obtain the desired product (29 g).

Aufarbeitung

  1. additionwas added dropwise
  2. customreaction at room temperature for 3 hours
  3. customCrystals thus precipitated
  4. filtrationwere collected by filtration
  5. temperatureheat-refluxed in 500 ml of ethyl acetate
  6. temperaturecooled
  7. customto precipitate
  8. filtrationfilter off solids
  9. concentrationThe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-9e5e9b55f683429fa89f2bf67ac707ea
Quelldatensatz
uspto-grants-1988_01
Patentnummer
US04719174

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