m-Chloroperbenzoic acid → HCID 135759112, compound

HRID 1995286Notes

Reaction equation

HRID 1995286 reaction equation
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3=[N:12][N:13]([CH3:15])[CH:14]=[C:9]3[C:8]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)=[N:7][C:6]=2[CH:23]=1.ClC1C=CC=C(C(OO)=[O:32])C=1>ClCCl>[OH2:32].[F:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3=[N:12][N:13]([CH3:15])[CH:14]=[C:9]3[C:8]([N:16]3[CH2:17][CH2:18][N+:19]([O-:32])([CH3:22])[CH2:20][CH2:21]3)=[N:7][C:6]=2[CH:23]=1

Participants

4

Reactant 2

HCID 70297m-Chloroperbenzoic acidHCID 135759099HCID 135759099, compound

Product 1

HCID 135759112HCID 135759112, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

7-Fluoro-2,10-dihydro-2-methyl-4-(4-methyl-1-piperazinyl)-pyrazolo[3,4-b][1,5]benzodiazepine (2.0 g) was stirred in dichloromethane (50 ml) at 0°-5° C. whilst m-chloroperbenzoic acid (1.5 g) was added in portions. The solution was stirred for 30 minutes then filtered through a column of basic alumina, eluting with 9:1 chloroform:methanol to give, after removal of the solvent and crystallisation from acetonitrile-diethyl ether, the title compound m.p. 228°.

Workup

  1. additionwas added in portions
  2. filtrationthen filtered through a column of basic alumina
  3. washeluting with 9:1 chloroform
  4. custommethanol to give
  5. customafter removal of the solvent and crystallisation from acetonitrile-diethyl ether

Sources & evidence

ORD record
ord-61bf2c7b2ae246b19797178ec35c7272
Source dataset
uspto-grants-1983_09
Patent number
US04404137

Reaction notes

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