Hydrochloric Acid → HCID 89838393, compound

HRID 1771144Notes

Reaction equation

HRID 1771144 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH2:24][CH3:25])=[C:17]([O:26][CH3:27])[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:28]>C(O)C>[ClH:28].[ClH:28].[CH3:22][O:21][C:19]1[CH:20]=[C:15]([CH:16]=[C:17]([O:26][CH3:27])[C:18]=1[O:23][CH2:24][CH3:25])[CH2:14][N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 89838174HCID 89838174, compound

Product 1

HCID 89838393HCID 89838393, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
20 °C

Procedure

To 4.1 g of N-(tert-butyloxycarbonyl)-N′-(3,5-dimethoxy-4-ethoxy-benzyl)piperazine 40 ml of 10% HCl and 10 ml of ethanol are added, the mixture is stirred for 5 h at 20° C., and evaporated to dryness in vacuum at 50÷80° C. Then 30 ml of dry acetone is added to the residue, the mixture is boiled with stifling for 20 min, cooled down to 10° C. White precipitate is filtered off in an hour, washed with 10 ml of acetone and dried at the air. The product (2 g) is used on the next step without further purification.

Workup

  1. customevaporated to dryness in vacuum at 50÷80° C
  2. additionThen 30 ml of dry acetone is added to the residue
  3. waitwith stifling for 20 min
  4. temperaturecooled down to 10° C
  5. filtrationWhite precipitate is filtered off in an hour
  6. washwashed with 10 ml of acetone
  7. customdried at the air
  8. customThe product (2 g) is used on the next step without further purification

Sources & evidence

ORD record
ord-a40756801be144b6a06407b25dbf9d30
Source dataset
uspto-grants-2016_02
Patent number
US09249115B2

Reaction notes

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