반응 #43386

반응 방정식

TBTU

DIPEA

(3-hydroxy-prop-1-yl)-piperidine

4-{2-[(5-chloro-thiophene-2-carbonyl)-amino]-2-methyl-propionylamino}-2-methyl-benzoic acid

DIPEA

→

5-chloro-thiophene-2-carboxylic acid-N-{1-methyl-1-[3-methyl-4-(2-{3-hydroxy-prop-1-yl}-piperidin-1-yl-carbonyl)-phenylcarbamoyl]-ethyl}-amide

용매

DMF

DMF

반응 조건

후처리

1. 1
   workup.ADDITIONmixed for 10 mins on a shaker
2. 2
   workup.ADDITIONagain mixed in
3. 3
   여과After 16 h at ambient temperature the mixture is filtered through basic aluminium oxide
4. 4
   세척washed with DMF/methanol=9:1
5. 5
   기타Then it is evaporated down i

실험 절차

200 μl of a 0.05 molar solution of 4-{2-[(5-chloro-thiophene-2-carbonyl)-amino]-2-methyl-propionylamino}-2-methyl-benzoic acid, which additionally contains 0.05 mol/l DIPEA, in DMF are combined with 100 μl of a 0.1-molar solution of TBTU in DMF on a microtitre plate and mixed for 10 mins on a shaker. Then 200 μl of a 0,05-molar solution of (3-hydroxy-prop-1-yl)-piperidine, which additionally contains 0.05 mol/l DIPEA, are pipetted in and again mixed in by shaking. After 16 h at ambient temperature the mixture is filtered through basic aluminium oxide and washed with DMF/methanol=9:1. Then it is evaporated down i. vac.

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