反应 #302893

ord-0a74d17aec6e4360a8b38730d97d3d46

反应方程式

Cc1cccc(CNC2=NCCS2)c1C.Cl
((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride
[Na+].[OH-]
sodium hydroxide
Cc1cccc(CNC2=NCCS2)c1C
title compound
收率 99.6%
Cc1cccc(CNC2=NCCS2)c1C
((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine
收率 99.6%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONThe reaction mixture was poured into a separatory funnel
  2. 2
    其他the organic phase was removed
  3. 3
    萃取The aqueous phase was extracted with 100 mL of diethyl ether
  4. 4
    萃取The organic extract
  5. 5
    干燥dried with sodium sulfite
  6. 6
    过滤filtered
  7. 7
    浓缩The filtrate was concentrated under reduced pressure

实验过程

A mixture of 1.4 grams (0.034 mole) of sodium hydroxide in 100 mL of water was added to a stirred, cold (ice water bath) mixture of 8.0 grams (0.031 mole) of ((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride (Compound C11) in 100 mL of diethyl ether. The reaction mixture was allowed to warm to ambient temperature where it stirred for two hours. The reaction mixture was poured into a separatory funnel and the organic phase was removed and saved. The aqueous phase was extracted with 100 mL of diethyl ether. The organic extract was combined with the saved organic phase, dried with sodium sulfite and filtered. The filtrate was concentrated under reduced pressure to yield 6.8 grams of the title compound as a white solid, melting point 110-114° C. The NMR spectrum was consistent with the proposed structure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08193118B2uspto-grants-2012_06