반응 #93946

ord-d525f170739548938a3dae54d1925a5f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도at reflux for 1 hour
  3. 3
    온도After cooling
  4. 4
    기타Crystallization from 25 ml of DMF
  5. 5
    기타gives 4.0 g (69%) of cream colored product, m.p. 243°-245°

실험 절차

A suspension of 4-[(4,5-dihydro-2-thiazolyl)amino]-tetrahydro-3,5-bis[(4-methoxyphenyl)methylene]thiopyran-4-ol-1,1-dioxide (6.0 g, 0.012 mole) in 75 ml of n-BuOH and 25 ml of DMSO is stirred and heated at reflux for 1 hour. The volume of the resulting solution is reduced by approximately one-half using a Dean-Stark trap. After cooling, the yield of yellow product is 4.7 g, m.p. 235°-240°. Crystallization from 25 ml of DMF gives 4.0 g (69%) of cream colored product, m.p. 243°-245°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04128647uspto-grants-1978_12