Hydrochloric Acid → HCID 89838555, compound

HRID 1771141Notes

Reaction equation

HRID 1771141 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:27]>C(O)C>[ClH:27].[ClH:27].[C:23]([C:17]1[CH:16]=[C:15]([CH:20]=[CH:19][C:18]=1[O:21][CH3:22])[CH2:14][N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)([CH3:26])([CH3:24])[CH3:25]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 89838245HCID 89838245, compound

Product 1

HCID 89838555HCID 89838555, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
20 °C

Procedure

To 3.5 g of N-(tert-butyloxycarbonyl)-N′-(3-tert-butyl-4-methoxy-benzyl)piperazine 30 ml of 10% HCl and 5 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 20 ml of dry acetone is added to the residue, the mixture is boiled with stifling for 20 min, then cooled down to 10° C. After 1 h the product is filtered off, washed with 10 ml of acetone and dried at the air. Yield of (3-tert-butyl-4-methoxybenzyl)piperazine dihydrochloride—2.2 g (68%).

Workup

  1. customevaporated to dryness in vacuum at 50÷80° C
  2. additionThen 20 ml of dry acetone is added to the residue
  3. waitwith stifling for 20 min
  4. temperaturecooled down to 10° C
  5. filtrationAfter 1 h the product is filtered off
  6. washwashed with 10 ml of acetone
  7. customdried at the air

Sources & evidence

ORD record
ord-67368a519c574fa89754209ca64bfb62
Source dataset
uspto-grants-2016_02
Patent number
US09249115B2

Reaction notes

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