반응 #2122513

ord-097b5858728d43679c2f44d922bf93e1

반응 방정식

Cc1nc2ccc(S(=O)(=O)Cl)cc2s1
Compound 2
Cc1nc2ccc(S(=O)(=O)Cl)cc2s1
2-methylbenzothiazole-6-sulfonyl chloride
C1CCNCC1
piperidine
CCCCCC
hexane
Cc1nc2ccc(S(=O)(=O)N3CCCCC3)cc2s1
Compound 3
수율 74.2%
Cc1nc2ccc(S(=O)(=O)N3CCCCC3)cc2s1
N-(2-methylbenzothiazole-6-sulfonyl)piperidine
수율 74.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml)
  2. 2
    건조The organic layer was dried with sodium sulfate
  3. 3
    기타evaporated
  4. 4
    기타The sticky white solid thus obtained
  5. 5
    기타The white solid that precipitated
  6. 6
    기타was collected
  7. 7
    세척washed with hexane
  8. 8
    기타dried

실험 절차

A solution of Compound 2 (2.5 g, 10 mmol) in chloroform (15 ml) was added drop wise to a solution of piperidine (1.7 g, 20.0 mmol) in chloroform (10 ml). The combined mixture was stirred at room temperature for 1 hour. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was dried with sodium sulfate and evaporated. The sticky white solid thus obtained was dissolved in ca. 5 ml of hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was collected, washed with hexane and dried to yield 2.2 g (74%) of Compound 3, Rf=0.28 (30% ethyl acetate in hexane). The structure of Compound 3 is given below:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08574881B2uspto-grants-2013_11