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ethyl (2R,3R)-3-{[(2S)-4-methyl-1-oxo-1-{4-[(2,3,4-trimethoxyphenyl)methyl]piperazin-1-yl}pentan-2-yl]carbamoyl}oxirane-2-carboxylate → HCID 23700901, Verbindung

HRID 1982503
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1982503
[OH-].[Na+:2].C(O)C.[CH3:6][CH:7]([CH3:42])[CH2:8][C@H:9]([NH:31][C:32]([C@@H:34]1[O:36][C@H:35]1[C:37]([O:39]CC)=[O:38])=[O:33])[C:10]([N:12]1[CH2:17][CH2:16][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=2[O:29][CH3:30])[CH2:14][CH2:13]1)=[O:11]>C(O)C>[CH3:6][CH:7]([CH3:42])[CH2:8][C@H:9]([NH:31][C:32]([C@@H:34]1[O:36][C@H:35]1[C:37]([O-:39])=[O:38])=[O:33])[C:10]([N:12]1[CH2:13][CH2:14][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=2[O:29][CH3:30])[CH2:16][CH2:17]1)=[O:11].[Na+:2]
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Komponenten

4

Edukt 2

HCID 6917749ethyl (2R,3R)-3-{[(2S)-4-methyl-1-oxo-1-{4-[(2,3,4-trimethoxyphenyl)methyl]piperazin-1-yl}pentan-2-yl]carbamoyl}oxirane-2-carboxylateHCID 23692425Sodium hydroxide ethanol

Produkt 1

HCID 23700901HCID 23700901, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Under cooling with ice, a 0.48N sodium hydroxide-ethanol solution (9.48 ml) was added to an ethanol solution (20 ml) of ethyl trans-3-[(s)-3-methyl-1-{4-(2,3,4-trimethoxyphenylmethyl)piperazine-1-yl carbonyl}butylcarbamoyl]-oxirane-2-carboxylate (2.38 g) obtained above, and the mixture was stirred at room temperature for 2.5 hours. After removal of ethanol by distillation under reduced pressure, water was added, and any insoluble matters were removed by filtration using sellaite. The filtrate was concentrated and dried under reduced pressure to yield 2.31 g of sodium trans-3-[(s)-3-methyl-1-{4-(2,3,4-trimethoxyphenylmethyl)piperazine-1-yl carbonyl}butylcarbamoyl]oxirane-2-carboxylate as a light yellow powder (yield: 98%).

Aufarbeitung

  1. temperatureUnder cooling with ice
  2. customobtained above, and the mixture
  3. customAfter removal of ethanol
  4. distillationby distillation under reduced pressure, water
  5. additionwas added
  6. customany insoluble matters were removed by filtration
  7. concentrationThe filtrate was concentrated
  8. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6ad4ab21b0094001a3aa9d4576c6fd20
Quelldatensatz
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04596803

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