Acetic Acid → HCID 86627515, 화합물

HRID 1970056노트

반응식

HRID 1970056 반응식
[I:1]Cl.[O:3]=[C:4]1[C:13]2[NH:14][CH:15]=[CH:16][C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[NH:5]1.[CH2:17]([C:19]([O-:21])=[O:20])[CH3:18].C(O)(=O)C.[O-]S(C(F)(F)F)(=O)=O.[In+3].[O-]S(C(F)(F)F)(=O)=O.[O-]S(C(F)(F)F)(=O)=O>ClCCl.C(#N)C>[I:1][C:9]1[CH:8]=[CH:7][C:6]2[NH:5][C:4](=[O:3])[C:13]3[NH:14][CH:15]=[CH:16][C:12]=3[C:11]=2[CH:10]=1.[CH2:17]([C:19]([O-:21])=[O:20])[CH3:18]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 24640Iodine chlorideHCID 2734680Indium(III) trifluoromethanesulfonateHCID 86627461HCID 86627461, 화합물

생성물 1

HCID 86627515HCID 86627515, 화합물수율 96%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

반응 조건

온도
45 °C

실험 절차

Alternatively, 1.5 mL (1.5 mmol) of a 1M solution of iodine monochloride in dichloromethane is added to a solution of 316 mg (1 mmol) of 4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-ethyl carboxylate cocrystallized with 1 equivalent of acetic acid and 652 mg (1 mmol) of indium triflate in anhydrous acetonitrile (20 mL). The solution is heated at 45° C. for 3 hours then stirred at room temperature for 20 hours. The solid is filtered, and triturated with acetonitrile and diisopropyl ether to give 368 mg (96%) of 8-iodo-4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-ethyl carboxylate in the form of a white solid.

후처리

  1. filtrationThe solid is filtered
  2. customtriturated with acetonitrile and diisopropyl ether

출처 및 근거

ORD 기록
ord-7deac5343834438e96cd7cc680ff0514
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426437B2

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