Ethyl acetate hexane → HCID 86702749, compound

HRID 2280082Notes

Reaction equation

HRID 2280082 reaction equation
[Si:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14](=[O:29])[C:15]#[C:16][CH2:17][CH2:18][CH2:19]/[CH:20]=[CH:21]/[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[Cl:28])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].CCOC(C)=O.CCCCCC>ClCCCl>[Si:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([C:15]1[C:27]2[C:22](=[C:23]([Cl:28])[CH:24]=[CH:25][CH:26]=2)[CH:21]=[C:20]2[CH2:19][CH2:18][CH2:17][C:16]=12)=[O:29])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 21226206Ethyl acetate hexaneHCID 86702750HCID 86702750, compound

Product 1

HCID 86702749HCID 86702749, compoundYield 97.4%

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Procedure

To a 10-20 mL microwave irradiation vial equipped with a stir bar was added compound 11 (0.35 g, 0.81 mmol) in DCE (13 mL). The reaction was irradiated with stirring at 180° C. for 180 min until complete by TLC (AcOEt/n-hexane 0.5:9.5). The solution turned golden in color. The mixture was then transferred to a vial, concentrated under reduced pressure, and dried under vacuum to yield the title compound as a brown oil (0.34 g, 97% yield).

Workup

  1. customTo a 10-20 mL microwave irradiation
  2. customvial equipped with a stir bar
  3. customThe reaction was irradiated
  4. concentrationconcentrated under reduced pressure
  5. customdried under vacuum

Sources & evidence

ORD record
ord-5cedc48e2f0a487cb662898f88132699
Source dataset
uspto-grants-2015_09
Patent number
US09133234B2

Reaction notes

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