Thiazole, 2-chloro-5-(2-chloroethyl)-4-methyl- → Clomethiazole

HRID 265642

反応式

HRID 265642 の反応式
Cl[C:2]1[S:3][C:4]([CH2:8][CH2:9][Cl:10])=[C:5]([CH3:7])[N:6]=1>[Pd].C(O)C>[CH3:7][C:5]1[N:6]=[CH:2][S:3][C:4]=1[CH2:8][CH2:9][Cl:10]

参加物

4

反応物 1

HCID 207964Thiazole, 2-chloro-5-(2-chloroethyl)-4-methyl-

生成物 1

HCID 10783Clomethiazole収率 91%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a solution of 63 g (0.32 moles) of 2-chloro-4-methyl-5-(2-chloroethyl)-thiazole in 630 cm3 of a 96% ethanol 9 g of a wet palladium on charcoal catalyst (palladium content: 8%) are added. The mixture is hydrogenated at atmospheric pressure. The termination of the reaction is indicated by the cease of the hydrogen consumption. After filtering off the catalyst the solution is evaporated, the residue is dissolved in water and the solution is neutralized with sodium hydrogen carbonate (pH 7). The separated oil is shaken out with chloroform. The residue after the evaporation of the chloroform solution is distilled under reduced pressure. 47 g (91%) of 4-methyl-5-(2-chloroethyl)-thiazole are obtained. Its boiling point is 105° C. at a pressure of 0.93 KPa, nD20 =1.5430. Its active agent content is 98.8%, determined by gas chromatography.

後処理

  1. customcease of the hydrogen consumption
  2. filtrationAfter filtering off the catalyst the solution
  3. customis evaporated
  4. dissolutionthe residue is dissolved in water
  5. customThe residue after the evaporation of the chloroform solution
  6. distillationis distilled under reduced pressure

出典と根拠

ORDレコード
ord-4a5508125f1d433e834989e53f13de22
出典データセット
uspto-grants-1997_07
特許番号
US05648498

関連ノート

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