Production method for 1,2,3,5,6-pentathiepane

Patent metadata

Field	Value
Publication number	US-11919877-B2
Application number	US-201916980030-A
Country	US
Kind code	B2
Filing date	Mar 5, 2019
Priority date	Mar 22, 2018
Publication date	Mar 5, 2024
Grant date	Mar 5, 2024

Abstract

The present invention enables provision of a production method for 1,2,3,5,6-pentathiepane, the method comprising, in the following order, step A for reacting a trithiocarbonate, sulfur, and a methane dihalide together using a phase-transfer catalyst in a multilayer system having a water layer and an organic layer, step B for separating the water layer from the organic layer, and step C for stopping the reaction using an acid.

First claim

The invention claimed is:

1. A method for producing 1,2,3,5,6-pentathiepane, the method comprising Steps A, B and C in this order:
Step A: reacting trithiocarbonate, sulfur and methane dihalide using a phase-transfer catalyst in a multi-layer system having an aqueous layer and an organic layer, wherein the multi-layer system is a two-layer system;
Step B: separating the aqueous layer from the organic layer; and
Step C: terminating the reaction with an acid,
wherein the method further comprises purifying 1,2,3,5,6-pentathiepane from the organic layer, after step C.

2. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the organic layer comprises one or more selected from the group consisting of benzene and toluene and tetrahydrofuran.

3. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the organic layer comprises toluene.

4. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the phase-transfer catalyst comprises a quaternary alkylammonium salt.

5. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the trithiocarbonate is disodium trithiocarbonate.

6. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the methane dihalide comprises dibromomethane or diiodomethane.

7. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the acid is sulfuric acid.

8. The method for producing 1,2,3,5,6-pentathiepane according to claim 1 , wherein the mass ratio of water and an organic solvent used in a solvent is in a range of 30:70-50:50.

Assignees

• Mitsubishi Gas Chemical Co

Inventors

• TANAGI Hiroyuki
• Takemura Kouhei
• Horikoshi Hiroshi

Classifications

• C07D341/00 Primary

  Heterocyclic compounds containing rings having three or more sulfur atoms as the only ring hetero atoms · CPC title

• B01J31/0239

  Quaternary ammonium compounds · CPC title

• B01J2531/98

  Phase-transfer catalysis in a mixed solvent system containing at least 2 immiscible solvents or solvent phases · CPC title

• C07B61/00

  Other general methods · CPC title

• B01J31/02

  containing organic compounds or metal hydrides · CPC title