p-Toluenesulfonic acid → HCID 131723764、化合物

HRID 1059046ノート

反応式

HRID 1059046 の反応式
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]

参加物

8

反応物 6

HCID 6101p-Toluenesulfonic acidHCID 5362487SulfurHCID 98341081,3-Dithiolane, 2-pentyl-HCID 12070523HCID 12070523、化合物HCID 57035733HCID 57035733、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 131723764HCID 131723764、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0bb27f2e35774abea7c25de39fa783bf
出典データセット
uspto-grants-2003_02
特許番号
US06518335B2

反応ノート

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