m-Chloroperbenzoic acid → HCID 70552863, compound

HRID 1106029Notes

Reaction equation

HRID 1106029 reaction equation
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][N:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[N:17]([C:24](=[O:33])[CH2:25][N:26]2[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]2)[C:16]2[N:34]=[C:35]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[N:36]=[CH:37][C:15]=2[C:14]1=[O:44]>CO>[CH3:12][N:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[N:17]([C:24](=[O:33])[CH2:25][N:26]2[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]2)[C:16]2=[N+:34]([O-:9])[C:35]([C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=3)=[N:36][CH:37]=[C:15]2[C:14]1=[O:44]

Participants

4

Reactant 2

HCID 70297m-Chloroperbenzoic acidHCID 20554362HCID 20554362, compound

Product 1

HCID 70552863HCID 70552863, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Conditions

Temperature
20 °C

Procedure

A solution of 0.7 g (3.4 mmol) of m-chloroperbenzoic acid (85 percent) in 10 ml of methanol is slowly added at room temperature to a suspension of 1 g (2,3 mmol) of 6-methyl-11-[(4-methyl-1-piperazinyl)acetyl]-2-phenyl-5,6-dihydropyrimido[4,5-b][1,5]benzodiazepin-5-one in 40 ml of methanol. After stirring for 3 hours at 20° C. and filtering, the filtrate is concentrated in vacuo and the residue is purified by chromatography on neutral silica gel using 20:1 chloroform/methanol as the eluant. Yield: 0.5 g (48%).

Workup

  1. filtrationfiltering
  2. concentrationthe filtrate is concentrated in vacuo
  3. customthe residue is purified by chromatography on neutral silica gel using 20:1 chloroform/methanol as the eluant

Sources & evidence

ORD record
ord-12cf69d623654882b17e7584f72da7d5
Source dataset
uspto-grants-1982_01
Patent number
US04311700

Reaction notes

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