Hydrazine → HCID 10113410, compound

HRID 1270185Notes

Reaction equation

HRID 1270185 reaction equation
ClC(Cl)(Cl)[C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19](=[O:32])[C:20]3[CH:25]=[CH:24][C:23]([CH:26]4[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]4)=[CH:22][CH:21]=3)[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4].[NH2:35][NH2:36]>C(O)C>[CH:26]1([C:23]2[CH:24]=[CH:25][C:20]([C:19]([N:10]3[C:11]4[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=4[CH2:13][N:14]4[C:5]([C:3]([NH:35][NH2:36])=[O:4])=[CH:6][CH:7]=[C:8]4[CH2:9]3)=[O:32])=[CH:21][CH:22]=2)[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]1

Participants

4

Reactant 2

HCID 9321HydrazineHCID 18449079HCID 18449079, compound

Product 1

HCID 10113410HCID 10113410, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2,2,2-Trichloro-1-[10-cyclohexyl-benzoyl]10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-1-ethanone of Example 7 (1.3 g) was added to a solution of anhydrous hydrazine (0.24 g) in absolute ethanol (50 mL). After stirring overnight at room temperature, the volatiles were removed in vacuo and the residue extracted with dichloromethane. The combined extracts were dried over anhydrous sodium sulfate and filtered through a short column of Magnesol®. Removal of the solvent provided the title compound as a pale yellow amorphous solid.

Workup

  1. customthe volatiles were removed in vacuo
  2. extractionthe residue extracted with dichloromethane
  3. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
  4. filtrationfiltered through a short column of Magnesol®
  5. customRemoval of the solvent

Sources & evidence

ORD record
ord-9ef7e0d09993498e8d2b1b7fdf188346
Source dataset
uspto-grants-2007_04
Patent number
US07202239B2

Reaction notes

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