HCID 67302202, compound → HCID 67301693, compound

HRID 643582Notes

Reaction equation

HRID 643582 reaction equation
O[Li].O.O.O.O.O.O.[O:9]=[C:10]1[N:16]([CH:17]2[CH2:22][CH2:21][N:20]([C:23]([O:25][C@@H:26]([C:36]([O:38]CC)=[O:37])[CH2:27][C:28]3[CH:33]=[CH:32][C:31]([Br:34])=[C:30]([Br:35])[CH:29]=3)=[O:24])[CH2:19][CH2:18]2)[CH2:15][CH2:14][C:13]2[CH:41]=[CH:42][CH:43]=[CH:44][C:12]=2[NH:11]1>O.C1COCC1>[O:9]=[C:10]1[N:16]([CH:17]2[CH2:22][CH2:21][N:20]([C:23]([O:25][C@@H:26]([C:36]([OH:38])=[O:37])[CH2:27][C:28]3[CH:33]=[CH:32][C:31]([Br:34])=[C:30]([Br:35])[CH:29]=3)=[O:24])[CH2:19][CH2:18]2)[CH2:15][CH2:14][C:13]2[CH:41]=[CH:42][CH:43]=[CH:44][C:12]=2[NH:11]1

Participants

5

Reactant 2

HCID 67302202HCID 67302202, compoundHCID 178526980HCID 178526980, compound

Product 1

HCID 67301693HCID 67301693, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of 210 mg (9 mmol) LiOH.6H2O in 40 mL water was added at RT to a solution of 3.64 g (5.83 mmol) of (R)-2-(3,4-dibromo-phenyl)-1-ethoxycarbonylethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 70 mL THF and the reaction mixture was stirred for 7 h at RT. The mixture was evaporated down i.vac., the residue was taken up in 100 mL water, 1 M HCl was added until an acid reaction was obtained, the precipitate was filtered off and dried in the vacuum drying chamber at 50° C. The product was reacted further without purification.

Workup

  1. customThe mixture was evaporated down i.vac
  2. addition1 M HCl was added until an acid reaction
  3. customwas obtained
  4. filtrationthe precipitate was filtered off
  5. customdried in the vacuum
  6. customdrying chamber at 50° C
  7. customThe product was reacted further without purification

Sources & evidence

ORD record
ord-4be63fc4dd3d40709f822192fb1c34a2
Source dataset
uspto-grants-2010_04
Patent number
US07700598B2

Reaction notes

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