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

HRID 265642노트

반응식

HRID 265642 반응식
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]

참가 물질

4

반응물 1

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

생성물 1

HCID 10783Clomethiazole수율 91%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4a5508125f1d433e834989e53f13de22
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648498

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