Propargyl alcohol → HCID 490484, 화합물

HRID 1068049노트

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HRID 1068049 반응식
[NH2:1][N:2]1[C:11]2[C:6](=[CH:7][C:8](I)=[CH:9][CH:10]=2)[C:5](=[O:13])[C:4]([C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)=[O:15])=[CH:3]1.[CH2:25]([OH:28])[C:26]#[CH:27]>C(NCC)C.C(O)C.[Cu]I.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[NH2:1][N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:27]#[C:26][CH2:25][OH:28])=[CH:9][CH:10]=2)[C:5](=[O:13])[C:4]([C:14]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)=[O:15])=[CH:3]1

참가 물질

7

반응물 2

HCID 7859Propargyl alcoholHCID 21192582HCID 21192582, 화합물

생성물 1

HCID 490484HCID 490484, 화합물

시약·촉매·용매 4

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매HCID 702Ethanol용매HCID 8021Diethylamine용매

실험 절차

1-Amino-N-(4-chlorobenzyl)-6-iodo-4-oxo-1,4-dihydro-3-quinolinecarboxamide (0.25 g) from Preparation No. 57, copper (I) iodide (32 mg), and bis(triphenylphosphine)palladium (II) chloride (19 mg) are suspended in diethylamine (8 mL). Propargyl alcohol (39 μL) is added and the mixture is allowed to stir at room temperature for 16 h. The mixture is diluted with ethanol and then concentrated in vacuo. The crude solid is triturated with dichloromethane and recrystallized in acetic acid to affording 76 mg of the title compound as a beige solid.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe crude solid is triturated with dichloromethane
  3. customrecrystallized in acetic acid

출처 및 근거

ORD 기록
ord-d2e24624b39a4e4cbd87d6ec85726602
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248739B1

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