Carbon Disulfide → HCID 18315100, compound

HRID 589230Notes

Reaction equation

HRID 589230 reaction equation
[CH2:1]([NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[O-2].[Zn+2:29].[C:30](=[S:32])=[S:31]>>[CH2:15]([N:14]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[C:30](=[S:31])[S-:32])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].[Zn+2:29].[CH2:15]([N:14]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[C:30](=[S:31])[S-:32])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]

Participants

4

Conditions

Temperature
70 °C

Procedure

To a 250 mL round bottomed flask was placed 76.5 g of ditridecylamine 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 a pale yellow liquid with a Zn content of 6.0%.

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-7c125232619b4e5eb6cfac3072619f2e
Source dataset
uspto-grants-2016_01
Patent number
US09228150B2

Reaction notes

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