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

Hydrochloric Acid → tert-butyl 3-[(1S)-1-hydroxypropyl]benzoate

HRID 1364316
Notes
Print preview

Reaction equation

HRID 1364316 reaction equation
C(N(CCCC)[C@H:6]([CH3:15])[C@H:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[OH:8])CCC.C(C1C=C(C=CC=1)[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])=O.C([Zn]CC)C.[Cl-].[NH4+].Cl>C1(C)C=CC=CC=1.CCCCCC>[OH:8][C@H:7]([C:9]1[CH:10]=[C:11]([CH:12]=[CH:13][CH:14]=1)[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:6][CH3:15]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 10845940Tert-butyl 3-formylbenzoateHCID 11003877(1S,2R)-(-)-2-(Dibutylamino)-1-phenyl-1-propanolHCID 178418750HCID 178418750, compound

Product 1

HCID 66934833tert-butyl 3-[(1S)-1-hydroxypropyl]benzoate
Yield 1,950.8%

Reagents, catalysts & solvents 2

HCID 1140TolueneSolventHCID 8058HexaneSolvent2×

Procedure

To the (1S,2R)-2-di-n-butylamino-1-phenyl-1-propanol (200 mg) in toluene (7 ml) solution, tert-butyl 3-formylbenzoate (3 g) in hexane (7 ml) solution was added and the mixture was stirred at room temperature for 20 minutes. Next, diethylzinc in 1N hexane solution (33 ml) was added to the reaction solution under ice cooling and the mixture was stirred at that temperature for 18 hours. Saturated ammonium chloride aqueous solution was added to the reaction solution, the mixture was stirred at 20 minutes, and 1N hydrochloric acid was added. The obtained mixed solution was extracted with ethyl acetate. The organic layer was dried over with anhydrous sodium sulfate, then concentrated to obtain the title compound (3.5 g).

Workup

  1. stirringthe mixture was stirred at that temperature for 18 hours
  2. stirringthe mixture was stirred at 20 minutes
  3. additionThe obtained mixed solution
  4. extractionwas extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over with anhydrous sodium sulfate
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-265d2a2fefc94ebb976ecf962c6d938e
Source dataset
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07888348B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes