Methanesulfonic Acid → HCID 19894523, compound

HRID 893010Notes

Reaction equation

HRID 893010 reaction equation
[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH2:16][CH2:15][CH2:14][CH2:13]3)[N:9]=[C:8]([N:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][OH:29])[CH2:19][CH2:18]3)[N:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:30][S:31](O)(=[O:33])=[O:32]>C(Cl)Cl.CCOCC.CCOCC>[CH3:30][S:31]([O:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][N:20]1[CH2:19][CH2:18][N:17]([C:8]2[N:7]=[C:6]([N:1]3[CH2:2][CH2:3][CH2:4][CH2:5]3)[N:11]=[C:10]([N:12]3[CH2:16][CH2:15][CH2:14][CH2:13]3)[N:9]=2)[CH2:22][CH2:21]1)(=[O:33])=[O:32]

Participants

5

Reactant 2

HCID 6395Methanesulfonic AcidHCID 19894627HCID 19894627, compound

Product 1

HCID 19894523HCID 19894523, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 21881112Ethyl ether methylene chlorideSolvent

Procedure

A mixture of 4-[4,6-bis(1-pyrrolidinyl)-1,3,5-triazin-2-yl]-1-piperazinehexanol (EXAMPLE 1, 1.22 g) in methylene chloride/ether (1/1, 30 ml) is mixed with a solution of methanesulfonic acid (0.28 g) in ether (15 ml). The mixture is concentrated and the residue crystallized twice from methanol/ether to give the title compound.

Workup

  1. concentrationThe mixture is concentrated
  2. customthe residue crystallized twice from methanol/ether

Sources & evidence

ORD record
ord-513513313d154d46b12243053eb29081
Source dataset
uspto-grants-1992_06
Patent number
US05120843

Reaction notes

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