Sodium Iodide → HCID 12852740, 화합물

HRID 1105883노트

반응식

HRID 1105883 반응식
Cl[C:2]1[S:6][N:5]([CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:4](=[O:15])[CH:3]=1.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.C(N(CC)CC)C.[I-].[Na+]>C(Cl)(Cl)Cl>[N:16]1([C:2]2[S:6][N:5]([CH2:7][CH2:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:4](=[O:15])[CH:3]=2)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 8082PiperidineHCID 8471TriethylamineHCID 13013787HCID 13013787, 화합물

생성물 1

HCID 12852740HCID 12852740, 화합물수율 20.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 2.4 g. (0.01 mole) of 5-chloro-2-phenethyl-4-isothiazolin-3-one, 0.85 g. (0.01 mole) of piperidine, 1.0 g. (0.01 mole) triethylamine and 0.1 g. sodium iodide in 10 ml of CHCl3 was heated under reflux for 18 hours. The mixture was washed with water, dried (MgSO4) and concentrated to dryness to give 2.7 g. of a liquid residue. This was purified by a dry column chromatography (11/2×20", silica gel, diisopropyl ether) to give 1.0 g. of a solid product, which was recrystallized from 100 ml of diisopropyl ether to give 0.6 g of the named product, mp 106°-108°.

후처리

  1. additionA mixture of 2.4 g
  2. temperatureunder reflux for 18 hours
  3. washThe mixture was washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated to dryness
  6. customto give 2.7 g
  7. customThis was purified by a dry column chromatography (11/2×20", silica gel, diisopropyl ether)
  8. customto give 1.0 g
  9. customof a solid product, which was recrystallized from 100 ml of diisopropyl ether

출처 및 근거

ORD 기록
ord-ec43ae4e90d94b37882f57c130439013
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04310590

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