تفاعل #80968

ord-9b91782861ca4dbb8947ac38a2842aa2

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated in vacuo
  2. 2
    تجفيفdried over Na2SO4
  3. 3
    تركيزconcentrated in vacuo
  4. 4
    أخرىPurification of the residue by silica gel chromatography

الإجراء التجريبي

A solution of 40 g of 4-(chloromethyl)-2-isopropylthiazole hydrochloride in 100 ml of water was added dropwise with stirring to 400 ml of 40% aqueous methylamine. The resulting solution was stirred for 1 h, then concentrated in vacuo. The residue was taken up in chloroform, dried over Na2SO4, and concentrated in vacuo. Purification of the residue by silica gel chromatography using 10% methanol in chloroform provided 21.35 g (55%) of the desired compound. 1H NMR (DMSO-d6) δ1.34 (d, J=7 Hz, 6H), 2.56 (s, 3H), 3.30 (heptet, J=7 Hz, 1H), 4.16 (s, 2H), 7.63 (s, 1H). Mass spectrum: (M+H)+ =171.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05616720uspto-grants-1997_04