Sulfuric Acid → Hexachlorobutadiene

HRID 46751

반응식

HRID 46751 반응식
ClC1(Cl)C(=O)C(Cl)=C1Cl.[Cl:10][C:11]1([Cl:19])[C:14]([Cl:15])=[C:13]([Cl:16])[C:12]1([Cl:18])[Cl:17].S(=O)(=O)(O)O.S(=O)(=O)=O>>[Cl:10][C:11]1([Cl:19])[C:14]([Cl:15])=[C:13]([Cl:16])[C:12]1([Cl:18])[Cl:17].[Cl:10][C:11]([Cl:19])=[C:14]([Cl:15])[C:13]([Cl:16])=[C:12]([Cl:18])[Cl:17]

참가 물질

6

반응물 4

HCID 1118Sulfuric Acid2회HCID 185452,3,4,4-Tetrachloro-2-cyclobuten-1-oneHCID 22504Hexachlorocyclobutene2회HCID 24682Sulfur trioxide2회

생성물 2

HCID 6901HexachlorobutadieneHCID 22504Hexachlorocyclobutene

실험 절차

Tetrachlorocyclobutenone, required as a starting material, is obtained with high yields and conversions by a not yet published process from hexachlorocyclobutene and a mixture of sulphuric acid and sulphur trioxide at elevated temperatures, e.g., by reaction of 1 mol hexachlorocyclobutene with approximately 1 mol each of sulphuric acid and sulphur trioxide at a temperature of 80° C. within 5 hours. Hexachlorocyclobutene can be obtained from hexachloro-1,3-butadiene in yields of near 100% of theory (DE-OS No. 26 18 557), corresponding to U.S. Pat. No. 4,115,460), for example by rectifying commercial hexachlorobutadiene at a pressure of from 2 to 100 mm Hg with a reflux ratio of from 300:1 to 600:1, subjecting hexachlorobutadiene remaining in the bottoms to a heat treatment at from 150° to 200° C. and then returning it to the rectifying column together with fresh commercial hexachlorobutadiene while withdrawing the product rich in hexachlorocyclobutene over the top. A suitable starting material is not only pure tetrachlorocyclobutenone but also crude tetrachlorocyclobutenone which may, for example, contain hexachlorobutadiene and hexachlorocyclobutene originating from its process of manufacture.

후처리

  1. customis obtained
  2. customwith high yields

출처 및 근거

ORD 기록
ord-836302dff01f4cb2b1919c94896ee549
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04175095

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