HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Boron tribromide → ethyl 5-(3,4-dihydroxy-5-nitrophenyl)-1-methyl-2-(2-(trifluoromethyl)pyridin-3-yl)-1H-pyrrole-3-carboxylate

HRID 62007
Notes
Print preview

Reaction equation

HRID 62007 reaction equation
C([O:8][C:9]1[CH:10]=[C:11]([C:26]2[N:30]([CH3:31])[C:29]([C:32]3[C:33]([C:38]([F:41])([F:40])[F:39])=[N:34][CH:35]=[CH:36][CH:37]=3)=[C:28]([C:42]([O:44][CH2:45][CH3:46])=[O:43])[CH:27]=2)[CH:12]=[C:13]([N+:23]([O-:25])=[O:24])[C:14]=1[O:15]CC1C=CC=CC=1)C1C=CC=CC=1.B(Br)(Br)Br>ClCCl>[OH:8][C:9]1[CH:10]=[C:11]([C:26]2[N:30]([CH3:31])[C:29]([C:32]3[C:33]([C:38]([F:41])([F:40])[F:39])=[N:34][CH:35]=[CH:36][CH:37]=3)=[C:28]([C:42]([O:44][CH2:45][CH3:46])=[O:43])[CH:27]=2)[CH:12]=[C:13]([N+:23]([O-:25])=[O:24])[C:14]=1[OH:15]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 25134Boron tribromideHCID 68701570HCID 68701570, compound

Product 1

HCID 68702622ethyl 5-(3,4-dihydroxy-5-nitrophenyl)-1-methyl-2-(2-(trifluoromethyl)pyridin-3-yl)-1H-pyrrole-3-carboxylate

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
-78 °C

Procedure

A solution of ethyl 5-(3,4-bis(benzyloxy)-5-nitrophenyl)-1-methyl-2-(2-(trifluoromethyl)pyridin-3-yl)-1H-pyrrole-3-carboxylate (0.189 g, 0.30 mmol) in dichloromethane (10 mL) was cooled to −78° C. with stirring and treated under argon with boron tribromide (0.30 g, 1.21 mmol). The resulting deep purple suspension was then allowed to stir at room temperature for one hour before cooling again to −78° C. The mixture was quenched by the careful addition of methanol. After stirring at room temperature for thirty minutes, the volatiles were evaporated and the residue stirred with 2 N hydrochloric acid (5 mL) for thirty minutes. The resulting solid was filtered off, washed with water (25 mL) and then cold isopropanol (5 mL) to give ethyl 5-(3,4-dihydroxy-5-nitrophenyl)-1-methyl-2-(2-(trifluoromethyl)pyridin-3-yl)-1H-pyrrole-3-carboxylate as a yellow solid, 0.126 g (93%).

Workup

  1. stirringto stir at room temperature for one hour
  2. customThe mixture was quenched by the careful addition of methanol
  3. stirringAfter stirring at room temperature for thirty minutes
  4. customthe volatiles were evaporated
  5. stirringthe residue stirred with 2 N hydrochloric acid (5 mL) for thirty minutes
  6. filtrationThe resulting solid was filtered off
  7. washwashed with water (25 mL)

Sources & evidence

ORD record
ord-37b58679fb494567940c125fdcb6b039
Source dataset
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09446012B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes