反応 #63026

ord-2f570d8df0f44c80ad9a8640ae3b2dba

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThroughout the addition
  2. 2
    workup.ADDITIONafter the completion of addition
  3. 3
    その他giving viscous colorless oil, which
  4. 4
    workup.ADDITIONupon addition of 50 ml
  5. 5
    その他of methanol precipitated 1.05 g

実験手順

To 1.8 g. of 1,4-diaminobutane dissolved in 50 ml. of H2O was added, dropwise, a solution of 2 g. of S-methylthiopseudourea.H2SO4 in 20 ml. of H2O. Throughout the addition, the solution was stirred vigorously and continued for 12 hours after the completion of addition. Then H2O was lyophilized, giving viscous colorless oil, which upon addition of 50 ml. of methanol precipitated 1.05 g. of white powder. Mass spec. (FD.) ions at m/e 228 and 130 for H2N--(CH2)4 --NHC(=NH)--NH2.H2O4 and H2N--(CH2)4 --NHC(=NH)--NH2, respectively.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04762949uspto-grants-1988_08