Hydrogen Sulfide → HCID 23347045, compound

HRID 1855939Notes

Reaction equation

HRID 1855939 reaction equation
[C:1]([CH2:3][CH2:4][Si:5]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8])#[N:2].C(NCC)C.[SH2:20]>>[CH2:13]([O:12][Si:5]([O:6][CH2:7][CH3:8])([O:9][CH2:10][CH3:11])[CH2:4][CH2:3][C:1]([NH2:2])=[S:20])[CH3:14]

Participants

4

Reactant 3

HCID 402Hydrogen Sulfide2×HCID 8021DiethylamineHCID 135223-(Triethoxysilyl)propionitrile

Product 1

HCID 23347045HCID 23347045, compound

Conditions

Temperature
60 °C

Procedure

Utilizing a 15 gallon high pressure stainless steel system, 80 pounds of beta-cyanoethyltriethoxysilane and 8 pounds of diethylamine were added initially. With a diptube, 12 pounds of hydrogen sulfide was charged into the reactor while cooling was maintained. The reactor was then heated to 60° C. with stirring for 6 hours. The residual hydrogen sulfide (80 psig) was carefully vented into a caustic scrubber and the product thioamide (94 pounds) was collected. The product, analyzed by InfraRed Spectroscopy, contained 5% unreacted nitrile.

Workup

  1. additionwere added initially
  2. temperaturewhile cooling
  3. temperaturewas maintained
  4. customthe product thioamide (94 pounds) was collected

Sources & evidence

ORD record
ord-cddf11bc723445ff8867fce67692c504
Source dataset
uspto-grants-1980_08
Patent number
US04217294

Reaction notes

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