Phosphorus pentachloride → HCID 21446958, compound

HRID 597187Notes

Reaction equation

HRID 597187 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]2[NH:8][C:9]3[C:15](=O)[N:14]([CH2:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[C:13]4[CH:24]=[CH:25][CH:26]=[CH:27][C:12]=4[O:11][C:10]=3[C:5]2=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[CH3:34][N:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1.[C:41]([OH:48])(=[O:47])/[CH:42]=[CH:43]/[C:44]([OH:46])=[O:45]>C(O)C>[C:41]([OH:48])(=[O:47])/[CH:42]=[CH:43]/[C:44]([OH:46])=[O:45].[CH2:17]([N:14]1[C:13]2[CH:24]=[CH:25][CH:26]=[CH:27][C:12]=2[O:11][C:10]2=[C:5]3[C:6](=[N:8][C:9]2=[C:15]1[N:38]1[CH2:39][CH2:40][N:35]([CH3:34])[CH2:36][CH2:37]1)[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4]3)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Participants

6

Reactant 4

HCID 24819Phosphorus pentachlorideHCID 531671-MethylpiperazineHCID 444972Fumaric AcidHCID 20381754HCID 20381754, compound

Product 1

HCID 21446958HCID 21446958, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

In the same way as described in example 1, 3-chloro-7-benzyl-7H-indolo[3,2-b][1,5]benzoxazepine-6(5H)-one, phosphorous pentachloride and N-methyl piperazine were reacted. The product was purified by chromatography on neutral alumina and elution with 3% ethanol in ether. The yellow oil thus obtained was reacted with fumaric acid in hot ethanol and the salt recrystallized from ethanol for analysis, mp. 217°-8°.

Workup

  1. customwere reacted
  2. customThe product was purified by chromatography on neutral alumina and elution with 3% ethanol in ether
  3. customThe yellow oil thus obtained
  4. customthe salt recrystallized from ethanol for analysis, mp. 217°-8°

Sources & evidence

ORD record
ord-76d3bc1d3b7e4c2e90b72a0d758ea4db
Source dataset
uspto-grants-1977_03
Patent number
US04013660

Reaction notes

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