Hydrochloric Acid → MLS002695130

HRID 993059Notes

Reaction equation

HRID 993059 reaction equation
[CH:1](=[C:8]1[C:13](=[O:14])[NH:12][C:11](=[O:15])[NH:10][C:9]1=[O:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+].O.Cl>CO>[CH2:1]([CH:8]1[C:9](=[O:16])[NH:10][C:11](=[O:15])[NH:12][C:13]1=[O:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

6

Procedure

To a suspension of 5-benzylidenebarbituric Acid (4 g) in 200 ml of methanol are added portionwise 1.4 g of sodium borohydride. After 10 minutes from the end of the addition, 100 ml of water are added and the mixture is acidified with 1 N hydrochloric acid to pH=2. The solvent is evaporated off and the aqueous phase is extracted with ethyl acetate. The pooled extracts are dried over sodium sulfate and concentrated to dryness. 3.6 g of the product crystallize, m.p. 207-209° C.

Workup

  1. additionare added
  2. customThe solvent is evaporated off
  3. extractionthe aqueous phase is extracted with ethyl acetate
  4. dry with materialThe pooled extracts are dried over sodium sulfate
  5. concentrationconcentrated to dryness
  6. custom3.6 g of the product crystallize

Sources & evidence

ORD record
ord-8fe768fe0fed4a3999ca21754de35712
Source dataset
uspto-grants-2002_10
Patent number
US06472396B1

Reaction notes

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