Diisopropylethylamine → HCID 57226830, Verbindung

HRID 1357866Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1357866
[CH3:1][C:2]1[C:7]2[N:8]=[C:9]([NH:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[O:10][C:6]=2[CH:5]=[C:4]([CH2:19][C:20](O)=[O:21])[CH:3]=1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C.[NH2:56][C:57]1[CH:62]=[CH:61][C:60]([C@H:63]([CH3:70])[CH2:64][C:65]([O:67][CH2:68][CH3:69])=[O:66])=[CH:59][CH:58]=1>CN(C)C=O.C(OCC)(=O)C>[CH3:1][C:2]1[C:7]2[N:8]=[C:9]([NH:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[O:10][C:6]=2[CH:5]=[C:4]([CH2:19][C:20]([NH:56][C:57]2[CH:58]=[CH:59][C:60]([C@H:63]([CH3:70])[CH2:64][C:65]([O:67][CH2:68][CH3:69])=[O:66])=[CH:61][CH:62]=2)=[O:21])[CH:3]=1

Komponenten

7

Edukt 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 18188094(4-Methyl-2-o-tolylamino-benzoxazol-6-yl)-acetic acidHCID 53963459HCID 53963459, Verbindung

Produkt 1

HCID 57226830HCID 57226830, VerbindungAusbeute 91,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A stirred solution of 2-(4-methyl-2-o-tolylaminobenzoxazol-6-yl)acetic acid [0.1 g, Reference Example 9(b)] in dimethylformamide (3 mL) was treated with O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (0.128 g), diisopropylethylamine (0.22 g) and after 5 minutes with ethyl (R) 3-(4-aminophenyl)butanoate (0.107 g, Reference Example 1). After 4 hours the reaction mixture was diluted with ethyl acetate and then washed with water, then with hydrochloric acid (1M), then twice with water, then with brine, then dried and then evaporated to give the title compound (0.15 g) as a brown oil.

Aufarbeitung

  1. washwashed with water
  2. dry with materialwith hydrochloric acid (1M), then twice with water, then with brine, then dried
  3. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d7ff232d3e9f4cb684f412885bcfbc24
Quelldatensatz
uspto-grants-2003_07
Patentnummer
US06593354B2

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