Hydrochloric Acid → 6-Amino-2-(butylamino)-9-(tetrahydro-3-furanylmethyl)-7,9-dihydro-8H-Purin-8-one hydrochloride salt

HRID 1011200Notes

Reaction equation

HRID 1011200 reaction equation
[NH2:1][C:2]1[N:10]=[C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:22])[N:6]2[CH2:16][CH:17]1[CH2:21][CH2:20][O:19][CH2:18]1.[ClH:23]>O1CCOCC1>[ClH:23].[NH2:1][C:2]1[N:10]=[C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:22])[N:6]2[CH2:16][CH:17]1[CH2:21][CH2:20][O:19][CH2:18]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 250251656-Amino-2-(butylamino)-9-(tetrahydro-3-furanylmethyl)-7,9-dihydro-8H-purin-8-one

Product 1

HCID 673145146-Amino-2-(butylamino)-9-(tetrahydro-3-furanylmethyl)-7,9-dihydro-8H-Purin-8-one hydrochloride salt

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

To 6-amino-2-(butylamino)-9-(tetrahydro-3-furanylmethyl)-7,9-dihydro-8H-purin-8-one (isomer 2) (1.2 g) at room temperature and under nitrogen was added 4.0M hydrochloric acid in 1,4-dioxane (12.73 ml) and the reaction stirred at for 30 minutes. The reaction was then concentrated in vacuo and left on the rotary evaporator for 2 hours at 50° C. The beige solid was recrystallised overnight from 2-butanone (18 ml). The crystals were collected by suction filtration and dried in vacuo at 50° C. for 30 minutes (960 mg).

Workup

  1. concentrationThe reaction was then concentrated in vacuo
  2. waitleft on the rotary evaporator for 2 hours at 50° C
  3. customThe beige solid was recrystallised overnight from 2-butanone (18 ml)
  4. filtrationThe crystals were collected by suction filtration
  5. customdried in vacuo at 50° C. for 30 minutes (960 mg)

Sources & evidence

ORD record
ord-4725f543b6ae403fbed23c5860abac1c
Source dataset
uspto-grants-2011_07
Patent number
US07977344B2

Reaction notes

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