반응 #5887

ord-a9b6c5936caf4afa829011ebb019f26e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After filtering off the solid
  2. 2
    기타the solution is evaporated
  3. 3
    기타to get a yellow solid which
  4. 4
    기타The solid separated
  5. 5
    추출is extracted with hexane
  6. 6
    여과filtered through 150 g of neutral alumina

실험 절차

To a stirred mixture of 75 g of 6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole and 29 g of sodium bicarbonate in 1100 ml of chloroform at 0° is added 41 g of thiophosgene and the mixture stirred at 10° for 4 hours. After filtering off the solid, the solution is evaporated to get a yellow solid which is dissolved in water and the pH of the solution is brought to 7 by the addition of dilute sodium hydroxide. The solid separated is extracted with hexane and filtered through 150 g of neutral alumina to give 2-tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole, melting at 124°-126°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246927uspto-grants-1993_09