Sodium Iodide → HCID 12852740、化合物

HRID 1105883ノート

反応式

HRID 1105883 の反応式
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

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 8082PiperidineHCID 8471TriethylamineHCID 13013787HCID 13013787、化合物

生成物 1

HCID 12852740HCID 12852740、化合物収率 20.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-ec43ae4e90d94b37882f57c130439013
出典データセット
uspto-grants-1982_01
特許番号
US04310590

反応ノート

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