N-methyl-2-pyrrolidone → HCID 131727974, compound

HRID 1175649Notes

Reaction equation

HRID 1175649 reaction equation
[C:1]([O:8][C:9]([C:12]([CH2:15][CH2:16]I)([F:14])[F:13])([F:11])[F:10])([C:4]([F:7])([F:6])[F:5])([F:3])[F:2].CN1CCCC1=[O:24]>O>[C:1]([O:8][C:9]([C:12]([CH2:15][CH2:16][OH:24])([F:14])[F:13])([F:11])[F:10])([C:4]([F:7])([F:6])[F:5])([F:3])[F:2]

Participants

4

Reactant 2

HCID 13387N-methyl-2-pyrrolidoneHCID 131727975HCID 131727975, compound

Product 1

HCID 131727974HCID 131727974, compoundYield 52%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

The flask was charged with 130 g of C2F5OCF2CF2CH2CH2I, 643 mL of the N-methyl pyrrolidone and 48 mL of deionized (DI) water. The reaction mixture was heated to 132 C for 20 hours. DI water was added and the lower layer was separated. The lower layer was dissolved in ether, washed with saturated sodium sulfite, and dried over anhydrous sodium sulfate. After rotary vaporization, 48 g of C2F5OCF2CF2CH2CH2OH (compound B3) was obtained by distillation in 52% yield. The boiling point was 70˜72° C. at 60 mm Hg pressure (7980 Pa).

Workup

  1. temperatureThe reaction mixture was heated to 132 C for 20 hours
  2. customthe lower layer was separated
  3. dissolutionThe lower layer was dissolved in ether
  4. washwashed with saturated sodium sulfite
  5. dry with materialdried over anhydrous sodium sulfate

Sources & evidence

ORD record
ord-882afb7d117c476aae9a5da89ef79aea
Source dataset
uspto-grants-2010_11
Patent number
US07842626B2

Reaction notes

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