Methylamine → HCID 53776622, compound

HRID 1837256Notes

Reaction equation

HRID 1837256 reaction equation
[CH3:1][NH2:2].[F:3][C:4]([F:24])([F:23])[C:5]([F:22])([F:21])[C:6]([F:20])([F:19])[C:7]([F:18])([F:17])[C:8]([F:16])([F:15])[C:9](F)([F:13])[CH2:10][CH2:11]I>O1CCCC1>[F:13][C:9]([C:8]([F:16])([F:15])[C:7]([F:18])([F:17])[C:6]([F:20])([F:19])[C:5]([F:22])([F:21])[C:4]([F:24])([F:23])[F:3])=[CH:10][CH2:11][NH:2][CH3:1]

Participants

4

Reactant 2

HCID 6329Methylamine2×HCID 748881,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

Product 1

HCID 53776622HCID 53776622, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

2.44 g of methylamine is condensed in a solution of 2.82 ml of 1,1,1,2,2,3,3,4,4,5,5,6,6 tridecafluor-8-iod-octane in 20 ml of anhydrous tetrahydrofuran at −40° C., and it is stirred overnight at room temperature in a pressurized reactor. After the pressurized reactor was opened at −30° C., it is allowed to come to room temperature to allow excess methylamine to evaporate off. Then, the reaction solution is mixed with diethyl ether, washed with saturated common salt solution, dried on magnesium sulfate and concentrated by evaporation in a vacuum. 2.23 g of (3,4,4,5,5,6,6,7,7,8,8,8-dodecafluor-oct-2-enyl)-methyl-amine is obtained as a crude product.

Workup

  1. customwas opened at −30° C.
  2. customto come to room temperature
  3. customto evaporate off
  4. additionThen, the reaction solution is mixed with diethyl ether
  5. washwashed with saturated common salt solution
  6. customdried on magnesium sulfate
  7. concentrationconcentrated by evaporation in a vacuum

Sources & evidence

ORD record
ord-404cce7ebcb749a7a846a30b4d6600ca
Source dataset
uspto-grants-2004_08
Patent number
US06780855B2

Reaction notes

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