反应 #1869178

反应方程式

compound

1-butyl-3-isobutyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

N,N-diisopropylethylamine

benzenesulfonylchloride resin

TsCl

6-phenylhexanol

→

title compound

收率 58.9%

1-butyl-3-isobutyl-8-(6-phenylhexyl)-1,3,8-triazaspiro[4.5]decane-2,4-dione hydrochloride

收率 58.9%

溶剂

acetonitrile

反应条件

后处理

1. 1
   过滤filtrated
2. 2
   洗涤The resin was washed with acetonitrile (3 mL, three times)
3. 3
   洗涤The filtrate and rinsed solution
4. 4
   浓缩concentrated
5. 5
   其他The residue was purified by column chromatography on silica gel (chloroform:methanol=25:1)
6. 6
   workup.ADDITIONadded 4N hydrochloric acid in ethyl acetate
7. 7
   浓缩concentrated

实验过程

To a solution of the compound prepared in Example 1 (28 mg) and N,N-diisopropylethylamine (155 mg) in acetonitrile (3 mL) were added benzenesulfonylchloride resin (Argonaut, product name PS-TsCl, product number 800276, 1.22 mmol/g, 0.20 mmol) (164 mg) and sulfonyl resin (175 mg) which is prepared from 6-phenylhexanol (345 mg). The mixture was stirred for 18 hours at 70° C. and then filtrated. The resin was washed with acetonitrile (3 mL, three times). The filtrate and rinsed solution were combined and concentrated. The residue was purified by column chromatography on silica gel (chloroform:methanol=25:1), added 4N hydrochloric acid in ethyl acetate and concentrated to give the title compound (28 mg) having the following physical data.

来源