p-Toluenesulfonic acid → HCID 70531396, compound

HRID 2166925Notes

Reaction equation

HRID 2166925 reaction equation
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:8][CH2:7]1.[NH2:17][N:18]1[C:27](=O)[C:26]2[C:21](=[CH:22][CH:23]=[C:24]([CH3:29])[CH:25]=2)[N:20]=[C:19]1NN.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[NH2:17][N:18]1[CH:27]=[C:26]2[C:21]([CH:22]=[CH:23][C:24]([CH3:29])=[CH:25]2)=[N:20][CH:19]1[NH:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][N:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:10][CH2:11]1

Participants

5

Reactant 3

HCID 6101p-Toluenesulfonic acidHCID 20497516Ethyl 4-(4-aminobutyl)piperazine-1-carboxylateHCID 20497519HCID 20497519, compound

Product 1

HCID 70531396HCID 70531396, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
180 °C

Procedure

A mixture of 10 g of ethyl 4-(4-aminobutyl)-piperazine-1-carboxylate, 5 g of 3-amino-2-hydrazino-6-methylquinazolin-4-(3H)-one and 0.5 g of p-toluenesulfonic acid was heated to 180° C. (bath temperature of reaction mixture 160° C.) for 4 hours. After cooling to 100° C., the reaction mixture was dissolved in 250 ml of toluene and was washed twice with 100 ml of water. The mixture filtered through `celite` and the product was retained in the toluene solution for use in the next stage.

Workup

  1. custom(bath temperature of reaction mixture 160° C.) for 4 hours
  2. temperatureAfter cooling to 100° C.
  3. washwas washed twice with 100 ml of water
  4. filtrationThe mixture filtered through `celite` and the product

Sources & evidence

ORD record
ord-e1130cb3cf364bbb989afda67dd83d35
Source dataset
uspto-grants-1983_06
Patent number
US04390697

Reaction notes

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