Iodine chloride → HCID 18940886, 화합물

HRID 356037노트

반응식

HRID 356037 반응식
[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]

참가 물질

4

반응물 2

HCID 24640Iodine chlorideHCID 45322241-Acetyl-6-chloroindoline

생성물 1

HCID 18940886HCID 18940886, 화합물수율 39%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-0272105375aa4e03a8e08330b830de25
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834494

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