Dioctylamine → HCID 14299313, compound

HRID 589232Notes

Reaction equation

HRID 589232 reaction equation
[CH2:1]([NH:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[O-2].[Zn+2:19].[C:20](=[S:22])=[S:21]>>[CH2:10]([N:9]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[C:20](=[S:21])[S-:22])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[Zn+2:19].[CH2:10]([N:9]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[C:20](=[S:21])[S-:22])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

Participants

4

Reactant 3

HCID 3094DioctylamineHCID 6348Carbon DisulfideHCID 3007857Zinc Oxide

Product 1

HCID 14299313HCID 14299313, compound

Conditions

Temperature
70 °C

Procedure

To a 250 mL round bottomed flask was placed 48.40 g of di-n-octylamine and 8.10 g of zinc oxide. Carbon disulfide, 16.0 g, was then added dropwise, and the mixture was stirred for 30 minutes. The flask was then stirred and heated for 2 hours at 70° C., and then stirred for an addition 2 hours at 90° C. A vacuum was then applied to remove water of reaction and the temperature was increased to 130° C., and the reaction was maintained in this state for 3 hours. The pale yellow material was then filtered through Celite at 120° C., to give, upon a pale yellow liquid with a Zn content of 8.1%.

Workup

  1. customTo a 250 mL round bottomed flask was placed
  2. stirringThe flask was then stirred
  3. stirringstirred for an addition 2 hours at 90° C
  4. customto remove
  5. customwater of reaction
  6. temperaturethe temperature was increased to 130° C.
  7. temperaturethe reaction was maintained in this state for 3 hours
  8. filtrationThe pale yellow material was then filtered through Celite at 120° C.

Sources & evidence

ORD record
ord-bbb80c4bee3a478e98a8d2f2240749d6
Source dataset
uspto-grants-2016_01
Patent number
US09228150B2

Reaction notes

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