Hydrochloric Acid → 1-(Methylsulfonyl)hoMopiperazine hydrochloride, 95%

HRID 2403459Notes

Reaction equation

HRID 2403459 reaction equation
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([S:15]([CH3:18])(=[O:17])=[O:16])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:19]>CO.CCOCC>[ClH:19].[CH3:18][S:15]([N:11]1[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]1)(=[O:16])=[O:17]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 220612771,1-Dimethylethyl hexahydro-4-(methylsulfonyl)-1H-1,4-diazepine-1-carboxylate

Product 1

HCID 174664531-(Methylsulfonyl)hoMopiperazine hydrochloride, 95%

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 3283Diethyl EtherSolvent

Procedure

Crude 4-methanesulfonyl-[1,4]diazepane-1-carboxylic acid tert-butyl ester (1.23 g) was stirred in anhydrous methanol (10 ml). 2M hydrogen chloride in ether (22 ml) was added. The reaction mixture was stirred at room temperature. After 5 minutes a precipitate formed, addition of anhydrous methanol (5 ml) caused this to dissolve. The reaction mixture was stirred overnight at room temperature. The solvents were removed in vacuo to yield 1.06 g of 1-methanesulfonyl-[1,4]diazepane hydrochloride salt.

Workup

  1. customAfter 5 minutes a precipitate formed
  2. dissolutionthis to dissolve
  3. stirringThe reaction mixture was stirred overnight at room temperature
  4. customThe solvents were removed in vacuo

Sources & evidence

ORD record
ord-0eb40535f58f4ccdb475e05323dde271
Source dataset
uspto-grants-2014_08
Patent number
US08802670B2

Reaction notes

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