Piperazine → HCID 53696522, compound

HRID 1283458Notes

Reaction equation

HRID 1283458 reaction equation
[Cl:1][C:2]1[C:3]([N:15]2[CH2:20][CH2:19][S:18](=[O:22])(=[O:21])[CH2:17][CH2:16]2)=[N:4][C:5](S(CC)(=O)=O)=[N:6][C:7]=1[C:8]#[N:9].[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>O1CCOCC1>[Cl:1][C:2]1[C:3]([N:15]2[CH2:16][CH2:17][S:18](=[O:21])(=[O:22])[CH2:19][CH2:20]2)=[N:4][C:5]([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)=[N:6][C:7]=1[C:8]#[N:9]

Participants

4

Reactant 2

HCID 4837PiperazineHCID 53804153HCID 53804153, compound

Product 1

HCID 53696522HCID 53696522, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

1.8 gm (0.005 mol) of 5-chloro-6-cyano-4-(1,1-dioxido-thiomorpholino)-2-ethylsulfonyl-pyrimidine (m.p. 234°-237°C, obtained from 2-ethylthio-5-chloro-6-cyano-4-thiomorpholino-pyrimidine by oxidation with potassium permanganate in dilute hydrochloric acid) were slowly added to a solution of 2.6 gm (0.03 mol) of piperazine in 50 ml of dioxane. After standing for a short time, the reaction solution was evaporated almost to dryness in vacuo, and the residue was taken up in about 50 ml of water. The insoluble reaction product was suction-filtered off, washed with water and dried. Yield: 1.4 gm (78% of theory).

Workup

  1. customthe reaction solution was evaporated almost to dryness in vacuo
  2. filtrationThe insoluble reaction product was suction-filtered off
  3. washwashed with water
  4. customdried

Sources & evidence

ORD record
ord-757cfd28c4db493bac8d016fcae8a9b3
Source dataset
uspto-grants-1976_08
Patent number
US03975384

Reaction notes

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