Hydrochloric Acid → HCID 19594629, compound

HRID 36658Notes

Reaction equation

HRID 36658 reaction equation
C([N:8]1[CH2:16][CH:15]2[CH:10]([NH:11][CH2:12][CH2:13][O:14]2)[CH2:9]1)C1C=CC=CC=1.[ClH:17]>CO.[Pd]>[ClH:17].[ClH:17].[CH:15]12[CH2:16][NH:8][CH2:9][CH:10]1[NH:11][CH2:12][CH2:13][O:14]2

Participants

5

Procedure

A solution of 4 g (18.2 mmol) of 8-benzyl-2-oxa-5,8-diazabicyclo[4.3.0]nonane in 100 ml of methanol and 3.5 ml of concentrated hydrochloric acid is hydrogenated on 2 g of palladium-on-active charcoal (10% of Pd) at 80° C. under 100 bar. The catalyst is filtered off and washed with water. The filtrates are concentrated and the product is crystallized by trituration with a little methanol. The crystals are filtered off with suction, washed with acetone and dried in air.

Workup

  1. filtrationThe catalyst is filtered off
  2. washwashed with water
  3. concentrationThe filtrates are concentrated
  4. customthe product is crystallized by trituration with a little methanol
  5. filtrationThe crystals are filtered off with suction
  6. washwashed with acetone
  7. customdried in air

Sources & evidence

ORD record
ord-f1973b60b0b14770b54b52dbe940f50b
Source dataset
uspto-grants-1995_05
Patent number
US05416096

Reaction notes

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