Hydrochloric Acid → HCID 20183530, Verbindung

HRID 255509Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 255509
[OH:1][C:2]1[C:10]([CH2:11][CH2:12][CH3:13])=[C:9]2[C:5]([CH:6]=[C:7]([C:14]([O:16]CC)=[O:15])[NH:8]2)=[CH:4][CH:3]=1.[C:19]([C:25](OC)=[O:26])#[C:20][C:21]([O:23]C)=[O:22].[OH-].[Na+].Cl>C(O)C.O>[O:26]=[C:25]1[C:3]2[CH:4]=[C:5]3[C:9](=[C:10]([CH2:11][CH2:12][CH3:13])[C:2]=2[O:1][C:20]([C:21]([OH:23])=[O:22])=[CH:19]1)[NH:8][C:7]([C:14]([OH:16])=[O:15])=[CH:6]3

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 12980Dimethyl acetylenedicarboxylateHCID 14798Sodium HydroxideHCID 20183534HCID 20183534, Verbindung

Produkt 1

HCID 20183530HCID 20183530, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The product of step (c) (0.6 g, 0.0024 M), dimethyl acetylene dicarboxylate (0.33 ml, 0.0027 M) and "Triton B" (2 drops) were heated under reflux for 6 hours in dry ethanol (10 ml). The reaction mixture was cooled, NaOH (0.6 g, 14.6 mmol) in water (6 ml) was added and refluxing continued for 1 hour. The whole was cooled, poured into dil. HCl, extracted into ethyl acetate and washed with brine before drying over MgSO4 and evaporating to dryness to yield the sub-title compound as a pale yellow solid, 0.7 g, (86%).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. temperaturerefluxing
  3. temperatureThe whole was cooled
  4. extractionextracted into ethyl acetate
  5. washwashed with brine
  6. dry with materialbefore drying over MgSO4
  7. customevaporating to dryness

Quellen und Nachweise

ORD-Eintrag
ord-e81a767ea03246699b9899c48f4b1a17
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04698345

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