Triethylamine → HCID 131722227, Verbindung

HRID 1275889Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1275889
[CH3:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]([C:16]3[C:17](=[S:32])[NH:18][C:19](=[O:31])[N:20]([CH2:22][C:23]4[S:24][CH:25]=[C:26]([C:28](O)=[O:29])[N:27]=4)[CH:21]=3)[C:7]3[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][C:8]=3[CH:9]=[CH:10][C:4]=2[CH:3]=1.[CH2:35]([O:37][C:38](=[O:46])[CH2:39][C:40]1[N:41]=[C:42]([NH2:45])[S:43][CH:44]=1)[CH3:36].F[P-](F)(F)(F)(F)F.Br[P+](N1CCCC1)(N1CCCC1)N1CCCC1.C(N(CC)CC)C>CN(C)C=O>[CH3:15][C:12]1[CH:13]=[CH:14][C:7]2[CH:6]([C:16]3[C:17](=[S:32])[NH:18][C:19](=[O:31])[N:20]([CH2:22][C:23]4[S:24][CH:25]=[C:26]([C:28]([NH:45][C:42]5[S:43][CH:44]=[C:40]([CH2:39][C:38]([O:37][CH2:35][CH3:36])=[O:46])[N:41]=5)=[O:29])[N:27]=4)[CH:21]=3)[C:5]3[CH:33]=[CH:34][C:2]([CH3:1])=[CH:3][C:4]=3[CH:10]=[CH:9][C:8]=2[CH:11]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 1044544-Thiazoleacetic acid, 2-amino-, ethyl esterHCID 2733179PyBroPHCID 221172312-[[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2-oxo-4-thioxo-1(2H)-pyrimidinyl]methyl]-4-thiazolecarboxylic acid

Produkt 1

HCID 131722227HCID 131722227, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The product from example 8(0.11 g) and 2-amino-4-thiazoleacetic acid ethyl ester (0.063 g) were dissolved in dry dimethylformamide (5 ml). Bromo-tris(pyrrolidino)-phosphonium hexafluorophosphate (0.11 g) and triethylamine (0.08 ml) were added and the mixture was stirred at room temperature for 24 hours. The reaction mixture was quenched with brine/HCl and extracted with ethyl acetate. The extract was washed with water, dried (MgSO4) and evaporated. The residue was purified by chromatography eluting with 10% ethyl acetate in dichloromethane and used directly in the next step.

Aufarbeitung

  1. customThe reaction mixture was quenched with brine/HCl
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by chromatography
  7. washeluting with 10% ethyl acetate in dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-3b64e6a53f9e49199d86902ef1ac3d21
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06162808

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