Hydrochloric Acid → HCID 68944694, compound

HRID 1984698Notes

Reaction equation

HRID 1984698 reaction equation
C(OC([NH:8][C@@H:9]([CH:20]([CH3:22])[CH3:21])[C:10]([C@H:12]1[C@H:16]([CH3:17])[C:15](=[O:18])[NH:14][C:13]1=[O:19])=[O:11])=O)(C)(C)C.[ClH:23]>O1CCOCC1>[ClH:23].[NH2:8][C@@H:9]([CH:20]([CH3:22])[CH3:21])[C:10]([C@H:12]1[C@H:16]([CH3:17])[C:15](=[O:18])[NH:14][C:13]1=[O:19])=[O:11]

Participants

4

Procedure

A solution cooled at 0° C. of 4.40 g (14.09 mmol) of (3R,4S)-3-[(2S)-2-(tert-butoxycarbonyl)amino-3-methylbutanoyl]-4-methyl-2,5-pyrrolidinedione (preparation: S. G. Davies, D. J. Dixon, J. Chem. Soc., Perkin Trans. 1, 1998, 17, 2635-2643) in 20 ml of dioxane is admixed dropwise with 35 ml of 4N hydrochloric acid solution in 1,4-dioxane. When the addition has been made the mixture is warmed to room temperature and stirred for 2 h, before being concentrated in vacuo. The residue is treated with diethyl ether. The precipitated crystals are filtered off and dried under a high vacuum. Yield: 2.99 g of colorless crystals (86% of theory).

Workup

  1. additionWhen the addition
  2. concentrationbefore being concentrated in vacuo
  3. additionThe residue is treated with diethyl ether
  4. filtrationThe precipitated crystals are filtered off
  5. customdried under a high vacuum

Sources & evidence

ORD record
ord-0cb11357a67249758dde04cc8a97d08a
Source dataset
uspto-grants-2009_06
Patent number
US07544709B2

Reaction notes

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