Water → HCID 68687571, compound

HRID 2244216Notes

Reaction equation

HRID 2244216 reaction equation
[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:6]=[CH:5][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[CH:20]=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:3][CH:2]=1.[Cl:29][C:30]([Cl:35])([Cl:34])[C:31](Cl)=[O:32].O>O1CCOCC1>[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:2]=[CH:3][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[C:20]([C:31](=[O:32])[C:30]([Cl:35])([Cl:34])[Cl:29])=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:5][CH:6]=1

Participants

5

Reactant 3

HCID 962WaterHCID 6420Trichloroacetyl chlorideHCID 9799174HCID 9799174, compound

Product 1

HCID 68687571HCID 68687571, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

10-(1,1′-Biphenyl-4-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step A (1.822 g; 0.005 mol) was dissolved in 50 mL of 1,4-dioxane to which was then added 0.946 g (0.0052 mol) of trichloroacetyl chloride. The reaction solution was heated under reflux with stirring over night, cooled to room temperature and then poured into 250 mL of water. Recrystallization of the crude material from ethanol provided a solid, m.p. 197-198° C.

Workup

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux
  3. customRecrystallization of the crude material from ethanol
  4. customprovided a solid, m.p. 197-198° C.

Sources & evidence

ORD record
ord-e83aa627fea141a297d2ee9749e36791
Source dataset
uspto-grants-2010_03
Patent number
US07678787B2

Reaction notes

Loading…