Methanol → HCID 10374752, compound

HRID 1766700Notes

Reaction equation

HRID 1766700 reaction equation
C([O:5][CH2:6][CH:7]([Cl:13])[CH2:8][C:9]([F:12])([F:11])[F:10])(=O)CC.CO.S(=O)(=O)(O)O>>[Cl:13][CH:7]([CH2:8][C:9]([F:12])([F:11])[F:10])[CH2:6][OH:5]

Participants

4

Reactant 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 86588502HCID 86588502, compound

Product 1

HCID 10374752HCID 10374752, compound

Procedure

2-Chloro-4,4,4-trifluorobutyl propionate (1) (9.58 g, 95.8 mmol), methanol (92 ml, 2.3 mol) and concentrated sulfuric acid (0.53 g, 10 mmol) are loaded into a 250-ml three-necked flask equipped with a condenser, a thermometer, a septum and a magnetic stirrer. The reaction medium is heated to reflux (between 60 and 65° C.). The mixture is left stirring for 2.5 hours. Distillation is performed at atmospheric pressure to remove the methanol and the methyl acetate. The residue is distilled at reduced pressure (38 mmHg).

Workup

  1. customequipped with a condenser
  2. temperatureThe reaction medium is heated
  3. temperatureto reflux (between 60 and 65° C.)
  4. waitThe mixture is left
  5. distillationDistillation
  6. customto remove the methanol
  7. distillationThe residue is distilled at reduced pressure (38 mmHg)

Sources & evidence

ORD record
ord-0eac2e8bb13a4c9a957a2c0a664e0e6d
Source dataset
uspto-grants-2007_06
Patent number
US07230147B2

Reaction notes

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