p-Toluenesulfonic acid → HCID 131723764, 화합물

HRID 1059046노트

반응식

HRID 1059046 반응식
C(C1SCCS1)CCCC.[S].C1(C)C=CC(S(O)(=O)=O)=CC=1.[H][H].CCCCCCSCCS.[CH3:35][O:36][Si:37]([O:47][CH3:48])([O:45][CH3:46])[CH2:38][CH2:39][CH:40]1[S:44][CH2:43][CH2:42][S:41]1>C1(C)C=CC=CC=1>[Si:37]([CH2:38][CH2:39][CH2:40][S:41][CH2:42][CH2:43][SH:44])([O:47][CH3:48])([O:36][CH3:35])[O:45][CH3:46]

참가 물질

8

반응물 6

HCID 6101p-Toluenesulfonic acidHCID 5362487SulfurHCID 98341081,3-Dithiolane, 2-pentyl-HCID 12070523HCID 12070523, 화합물HCID 57035733HCID 57035733, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 131723764HCID 131723764, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Into a 300 ml rocking autoclave were charged 58.2 g (0.331 m) of 2-(n-pentyl)-1,3-dithiolane, 1.06 g of sulfur, 0.12 g of p-toluenesulfonic acid, and 1.87 g of cobalt polysulfide catalyst (added as a 43% slurry in toluene). The autoclave was pressurized with hydrogen and maintained between 1600 and 2200 psi while being heated to 250°. After cooling and venting, the crude product contained 57% of the hydrogenolysis product, CH3(CH2)5S(CH2)2SH, as determined by GC/MS. When this procedure is applied to the product of Example 1, the hydrogenolysis product, (MeO)3Si(CH2)3S(CH2)2SH, is obtained.

후처리

  1. temperaturemaintained between 1600 and 2200 psi
  2. temperaturewhile being heated to 250°
  3. temperatureAfter cooling

출처 및 근거

ORD 기록
ord-0bb27f2e35774abea7c25de39fa783bf
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06518335B2

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