Methyl Isocyanate → HCID 73676698, compound

HRID 616167Notes

Reaction equation

HRID 616167 reaction equation
[N:1](=[C:3]1[S:8][CH2:7][S:6][CH2:5][S:4]1)[OH:2].[CH3:9][N:10]=[C:11]=[O:12]>CC(C)=O.C(N(CC)CC)C>[CH3:9][NH:10][C:11]([CH:7]1[S:8][C:3](=[N:1][OH:2])[S:4][CH2:5][S:6]1)=[O:12]

Participants

5

Reactant 2

HCID 12228Methyl IsocyanateHCID 204370381,3,5-Trithian-2-one, oxime

Product 1

HCID 73676698HCID 73676698, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 8471TriethylamineSolvent

Procedure

A quantity of 3.3 g of 2-oximino-1,3,5-trithiane and 1.29 ml of methyl isocyanate were dissolved in 50 ml of acetone containing 0.05 ml of triethylamine in a glass pressure vessel. The reaction mixture was allowed to stand for 72 hours at ambient temperature. The solvent was then evaporated and the residue taken up in 200 ml of ethyl acetate. The solution was washed with water, dried over magnesium sulfate and the solvent evaporated off. Recrystallization from isopropyl ether/acetone yielded 2.47 g of 2-methylcarbamoyloximino-1,3,5-trithiane, mp 129°-130°. The compound is identical in spectral properties to that obtained in Example II.

Workup

  1. customThe solvent was then evaporated
  2. washThe solution was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent evaporated off
  5. customRecrystallization from isopropyl ether/acetone

Sources & evidence

ORD record
ord-0131eb7953f9461e92bce1d4fbb52dcc
Source dataset
uspto-grants-1978_02
Patent number
US04072750

Reaction notes

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