Hydrochloric Acid → HCID 70578051, Verbindung

HRID 225305

Reaktionsgleichung

Reaktionsgleichung von HRID 225305
[NH2:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[C:3]([OH:5])=[O:4].[ClH:13].[CH2:14]=O>CO>[ClH:13].[NH2:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([CH2:14][Cl:13])[CH:7]=1)[C:3]([OH:5])=[O:4]

Komponenten

5

Edukt 3

HCID 313Hydrochloric Acid2×HCID 712FormaldehydeHCID 921434-Hydroxyphenylglycine

Produkt 1

HCID 70578051HCID 70578051, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of (-)-α-amino-4-hydroxybenzeneacetic acid (100 g, 0.6 mole) in a minimum amount of concentrated hydrochloric acid at 35°-40° C. is added 50 ml of aqueous formaldehyde (35-37%) (0.6 mole). The addition of hydrogen chloride gas is begun. After 5-10 minutes, a solid begins to precipitate. Stirring is continued for 30 minutes, and the solid is then collected. The crude product is washed with ether and with acetone. A second crop is obtained from the filtrate after standing at room temperature overnight. Total yield is 102 g (67%) m.p. >300° C., [α]D18 =-134° (c 4.75, CH3OH) NMR (DMSO-D6) ppm (δ) 4.68 (s,2), 4.9 (broad s,1), 6.9-7.6 (superimposed q and s,3).

Aufarbeitung

  1. customto precipitate
  2. waitis continued for 30 minutes
  3. customthe solid is then collected
  4. washThe crude product is washed with ether and with acetone
  5. customA second crop is obtained from the filtrate
  6. waitafter standing at room temperature overnight

Quellen und Nachweise

ORD-Eintrag
ord-5af12cd787af44039489c0a8ab470093
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04236002

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