反应 #40345

ord-fecbe090558448a4a06f30a565bfc4fc

反应方程式

CCN(C(C)C)C(C)C
Diisopropylethylamine
C=CCC(=O)O
vinyl acetic acid
CN(C)[P+](Oc1cccc2[nH]nnc12)(N(C)C)N(C)C.F[P-](F)(F)(F)(F)F
benzotriazolyloxy-tris-(dimethylamino)phosphonium hexafluorophosphate
Cl.Cl.N=C(N)Nc1nc2c(s1)CNCC2
N-(4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine-2-yl)-guanidine-dihydrochloride
[Na+].[OH-]
caustic soda
C=CCC(=O)N1CCc2nc(NC(=N)N)sc2C1
title compound
C=CCC(=O)N1CCc2nc(NC(=N)N)sc2C1
N-(5-but-3-enoyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine-2-yl)-guanidine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extraction with ethyl acetate

实验过程

Diisopropylethylamine (0.22 mmol), vinyl acetic acid (0.11 mmol) and benzotriazolyloxy-tris-(dimethylamino)phosphonium-hexafluorophosphate (0.11 mmol) are added successively to a stirred suspension of N-(4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine-2-yl)-guanidine-dihydrochloride (0.1 mmol) in dimethylformamide (0.7 mL), and the reaction mixture is stirred for 16 hours at room temperature. After the addition of 2M caustic soda solution (1 ml) there is extraction with ethyl acetate. The combined organic phases produce the pure title compound after drying over sodium sulphate and concentrating to dryness.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727979B2uspto-grants-2010_06