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Methacrylic Acid → 8-(2,6-Dichlorobenzoylamino)-4-(2-methacryloylhydrazino)quinoline

HRID 613549
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HRID 613549 반응식
[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH2:18])=[O:5].[C:24](O)(=[O:28])[C:25]([CH3:27])=[CH2:26].ON1C2C=CC=CC=2N=N1>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH:18][C:24](=[O:28])[C:25]([CH3:27])=[CH2:26])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 4093Methacrylic AcidHCID 757711-HydroxybenzotriazoleHCID 19592850HCID 19592850, 화합물

생성물 1

HCID 195923738-(2,6-Dichlorobenzoylamino)-4-(2-methacryloylhydrazino)quinoline수율 79.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857
Ethyl Acetate
용매

실험 절차

A mixture of 8-(2,6-dichlorobenzoylamino)-4-hydrazinoquinoline (200 mg), methacrylic acid (54.5 mg), 1-ethyl-3-(3-dimethylaminopropyl)-arbodiimide hydrochloride (133 mg) and 1-hydroxybenzotriazole (93.4 mg) in dimethylformamide (4 ml) was stirred for 4.5 hours at ambient temperature. The mixture was diluted with ethyl acetate and washed with water, saturated sodium bicarbonate solution and brine. The insoluble materials were collected by filtration and recrystallized from ethanol to give 8-(2,6-dichlorobenzoylamino)-4-(2-methacryloylhydrazino)quinoline (190 mg).

후처리

  1. washwashed with water, saturated sodium bicarbonate solution and brine
  2. filtrationThe insoluble materials were collected by filtration
  3. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-19c50daefb4f464eb0ab9ba740ab7ccb
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06008230

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