p-Toluenesulfonic acid monohydrate → HCID 2772320, compound

HRID 2082132Notes

Reaction equation

HRID 2082132 reaction equation
Cl.Cl.[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][CH2:18][N:19]2[C:25](=[O:26])[CH:24]3[C:27]([CH3:29])([CH3:28])[C:21]([CH3:30])([CH2:22][CH2:23]3)[C:20]2=[O:31])[CH2:11][CH2:10]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CCOCC>[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][CH2:18][N:19]2[C:25](=[O:26])[CH:24]3[C:27]([CH3:28])([CH3:29])[C:21]([CH3:30])([CH2:22][CH2:23]3)[C:20]2=[O:31])[CH2:13][CH2:14]1

Participants

4

Reactant 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 19779652HCID 19779652, compound

Product 1

HCID 2772320HCID 2772320, compoundYield 186.2%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To a solution of 0.399 g (0.001 mol) of compound I obtained according to Example 2, in 5 ml of iospropyl alcohol, there was added a solution of 0.38 g (0.002 mol) of p-toluenesulphonic acid monohydrate in 3 ml of the same solvent. The mixture was thoroughly mixed, and 40 ml of absolute ether was added thereto. The precipitated ditosylate was filtered off and dried in vacuum to yield 0.742 g (~100%) of the product. Mp. 137°-138° C.

Workup

  1. additionThe mixture was thoroughly mixed
  2. filtrationThe precipitated ditosylate was filtered off
  3. customdried in vacuum

Sources & evidence

ORD record
ord-2fa72101a6f448aaafbecd347f2c9446
Source dataset
uspto-grants-1993_02
Patent number
US05187277

Reaction notes

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