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

Sulfuric Acid → 3-Methylcyclopentadecene-1-yl acetate

HRID 2260928
Notes
Print preview

Reaction equation

HRID 2260928 reaction equation
P(OC1C=CC=CC=1)(OC1C=CC=CC=1)(OC1C=CC=CC=1)=O.C[Zn]C.[C:27]([O:30][C:31](=[O:33])[CH3:32])(=O)[CH3:28].[C:34]1(=O)[CH2:48][CH2:47]C[CH2:45][CH2:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH2:38][CH2:37][CH:36]=[CH:35]1.S(=O)(=O)(O)O>C(S([O-])(=O)=O)(F)(F)F.C(S([O-])(=O)=O)(F)(F)F.[Cu+2].C1(C)C=CC=CC=1>[C:31]([O:30][C:27]1[CH2:47][CH2:48][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH:44]([CH3:45])[CH:28]=1)(=[O:33])[CH3:32]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 8289Triphenyl PhosphateHCID 540403452-CyclopentadecenoneHCID 178477796HCID 178477796, compound

Product 1

HCID 687753723-Methylcyclopentadecene-1-yl acetateYield 92%

Reagents, catalysts & solvents 2

HCID 2734996copper(II) trifluoromethanesulfonateCatalystHCID 1140TolueneSolvent2×

Conditions

Temperature
25 °C

Procedure

Placed in a 2000-mL flask equipped with a stirrer, dropping funnel and thermometer were 54.3 mg (0.15 mmol) of Cu(OTf)2, 25 g of toluene and 93.1 mg (0.30 mmol) of triphenyl phosphate, and the inner atmosphere was replaced with nitrogen. After replacement with nitrogen, the mixture was stirred at 25° C. for 20 min. Then, 9 mL (18 mmol) of a toluene solution (2.0 mmol/L) of dimethylzinc was added to the mixture at 25° C., followed by further stirring for 10 min. The mixture was then cooled to −17° C., followed by addition of 1.68 g (16.5 mmol) of acetic anhydride, and 3.34 g (15 mmol) of 2-cyclopentadecenone was added dropwise to the mixture over the period of 1 hour. After completion of the dropwise addition, stirring was continued at the same temperature for 6 hours. After the reaction was completed, 32.5 g of a 5% aqueous sulfuric acid solution as cooled to 0° C. was added to the reaction mixture for quenching. After separation, the organic layer was washed with water (5 times), and the resultant organic layer was concentrated under reduced pressure to give 4.93 g of a crude product. The crude product was purified by silica-gel column chromatography to produce 3.89 g (13.8 mmol, 92% yield) of dl-3-methycyclopentadecene-1-yl acetate.

Workup

  1. customPlaced in a 2000-mL flask
  2. customequipped with a stirrer
  3. stirringby further stirring for 10 min
  4. temperatureThe mixture was then cooled to −17° C.
  5. additionwas added dropwise to the mixture over the period of 1 hour
  6. additionAfter completion of the dropwise addition
  7. stirringstirring
  8. waitwas continued at the same temperature for 6 hours
  9. additionwas added to the reaction mixture
  10. customfor quenching
  11. customAfter separation
  12. washthe organic layer was washed with water (5 times)
  13. concentrationthe resultant organic layer was concentrated under reduced pressure
  14. customto give 4.93 g of a crude product
  15. customThe crude product was purified by silica-gel column chromatography

Sources & evidence

ORD record
ord-795cf151034845a4ac043124c056d6c5
Source dataset
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07846701B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes