Iodine chloride → HCID 18940886、化合物

HRID 356037ノート

反応式

HRID 356037 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[I:14]Cl>C(O)(=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([I:14])=[C:10]([Cl:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 24640Iodine chlorideHCID 45322241-Acetyl-6-chloroindoline

生成物 1

HCID 18940886HCID 18940886、化合物収率 39%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1-Acetyl-6-chloroindoline (0.3 g, 1.53 mmol) and iodine monochloride (2.48 g, 15.3 mmol) in acetic acid (25 ml) were heated under reflux for 48 hours. After cooling the mixture was partitioned between ethyl acetate and 10% aqueous NaOH. The organic extract was washed with aqueous Na2 SO3 dried (Na2SO4) & evaporated to dryness under reduced pressure. Chromatography on silica gel using dichloromethane afforded the title compound (0.19 g, 39%).

後処理

  1. temperatureunder reflux for 48 hours
  2. temperatureAfter cooling the mixture
  3. customwas partitioned between ethyl acetate and 10% aqueous NaOH
  4. extractionThe organic extract
  5. washwas washed with aqueous Na2
  6. dry with materialSO3 dried (Na2SO4)
  7. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-0272105375aa4e03a8e08330b830de25
出典データセット
uspto-grants-1998_11
特許番号
US05834494

反応ノート

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