Hydrogen Sulfide → HCID 14447407, Verbindung

HRID 1973076Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1973076
[C:1]1([CH:7]([C:9]([O:11][CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O[CH:28]=[S:29])C.S>O1CCCC1>[S:29]=[CH:28][NH:8][CH:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:9]([O:11][CH:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)=[O:10]

Komponenten

5

Edukt 3

HCID 402Hydrogen SulfideHCID 11073343Methanethioic acid, O-ethyl esterHCID 131710294HCID 131710294, Verbindung

Produkt 1

HCID 14447407HCID 14447407, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 15.9 g. (0.05 mol.) of α-phenylglycine, diphenylmethyl ester, and 9 g. (0.01 mol.) of ethylthioformate in 50 ml. of tetrahydrofuran is stirred overnight at room temperature. Then a stream of hydrogen sulfide is passed into the solution for ten minutes, the reaction mixture is permitted to stand overnight, then concentrated and petroleum ether is added to the residue. 16.9 g. of α-[(thioxomethyl)-amino]benzeneacetic acid, diphenylmethyl ester, crystallizes. The crude product is recrystalized from methanol, m.p. 129°-130°.

Aufarbeitung

  1. concentrationconcentrated
  2. additionpetroleum ether is added to the residue
  3. customof α-[(thioxomethyl)-amino]benzeneacetic acid, diphenylmethyl ester, crystallizes
  4. customThe crude product is recrystalized from methanol, m.p. 129°-130°

Quellen und Nachweise

ORD-Eintrag
ord-27ecc21f828f43b39bcfeb7d3ef8f7d5
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03996219

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