Water → HCID 53937887, compound

HRID 1283461Notes

Reaction equation

[Mn]([O-])(=O)(=O)=[O:2].[K+].[CH3:7][C:8]1[N:13]=[C:12]([N:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[N:11]=[C:10]([N:20]2[CH2:25][CH2:24][S:23][CH2:22][CH2:21]2)[C:9]=1[N+:26]([O-:28])=[O:27].[OH2:29]>Cl>[CH3:7][C:8]1[N:13]=[C:12]([N:14]2[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]2)[N:11]=[C:10]([N:20]2[CH2:21][CH2:22][S:23](=[O:2])(=[O:29])[CH2:24][CH2:25]2)[C:9]=1[N+:26]([O-:28])=[O:27]

Participants

Conditions

Temperature: 5 °C

Procedure

A solution of 0.8 gm (0.005 mol) of potassium permanganate in 30 ml of water was slowly added dropwise to a solution of 1.6 gm (0.005 mol) of 6-methyl-5-nitro-2-piperazino-4-thiomorpholino-pyrimidine (m.p. 141°-142°C) in about 60 ml of 0.5 N hydrochloric acid at about 5°C. After stirring the reaction mixture for 1 hour at about 5°C, the precipitated manganese dioxide was removed by means of a sodium bisulfite solution. The reaction product was precipitated by addition of concentrated ammonia, washed with water and dried (m.p. 208°-211°C). Yield: 1.4 gm (79% of theory).

Workup

customthe precipitated manganese dioxide was removed by means of a sodium bisulfite solution
customThe reaction product was precipitated by addition of concentrated ammonia
washwashed with water
customdried (m.p. 208°-211°C)

Sources & evidence

ORD record: ord-2606bc8f24bf40319b2c3771fc67878c
Source dataset: uspto-grants-1976_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US03975384

Reaction notes

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