Water → HCID 20346994, compound

HRID 1701565Notes

Reaction equation

HRID 1701565 reaction equation
[CH:1]1([C:7]2[CH:13]=[C:12]([CH2:14][CH3:15])[C:10]([NH2:11])=[C:9]([CH2:16][CH3:17])[CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.C(=O)([O-])[O-].[Ca+2].[C:24](Cl)(Cl)=[S:25]>C(Cl)Cl>[CH:1]1([C:7]2[CH:8]=[C:9]([CH2:16][CH3:17])[C:10]([N:11]=[C:24]=[S:25])=[C:12]([CH2:14][CH3:15])[CH:13]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

6

Reactant 4

HCID 962WaterHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 20346919HCID 20346919, compound

Product 1

HCID 20346994HCID 20346994, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

231 g of 4-cyclohexyl-2,6-diethyl-aniline in 300 ml of methylene chloride are added dropwise at 10°-15° C. to a suspension of 600 ml of methylene chloride, 500 ml of water, 200 g of calcium carbonate and 140 g of thiophosgene. The mixture is then heated to the boil, until the evolution of gas has ended. The batch, when cold, is filtered to remove solids, and the methylene chloride layer is dried over calcium chloride and fractionated; boiling point 175°-179° C./1.5 mm Hg; yield 251 g.

Workup

  1. temperatureThe mixture is then heated to the boil, until the evolution of gas
  2. filtrationThe batch, when cold, is filtered
  3. customto remove solids
  4. dry with materialthe methylene chloride layer is dried over calcium chloride

Sources & evidence

ORD record
ord-ef6ca0d802074096a6ce77bbf5ca17e9
Source dataset
uspto-grants-1980_03
Patent number
US04194008

Reaction notes

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