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Oxalic Acid → (E)-2-[2-(Cyclohexyl)ethenyl]-5-methyl-1-(2-pyridyl)-1H-benzimidazole oxalate

HRID 382573
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HRID 382573 반응식
[CH3:1][C:2]1[CH:14]=[CH:13][C:5]([NH:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:4]([NH2:15])[CH:3]=1.[CH:16]1(/[CH:22]=[CH:23]/[C:24](Cl)=O)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.N1C=CC=CC=1N1C2C=CC=CC=2N=C1/C=C/C1C=CC=CC=1.[C:50]([OH:55])(=[O:54])[C:51]([OH:53])=[O:52]>C(OCC)(=O)C>[C:50]([OH:55])(=[O:54])[C:51]([OH:53])=[O:52].[CH:16]1(/[CH:22]=[CH:23]/[C:24]2[N:6]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=3)[C:5]3[CH:13]=[CH:14][C:2]([CH3:1])=[CH:3][C:4]=3[N:15]=2)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1
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참가 물질

6

반응물 4

HCID 971Oxalic AcidHCID 9796241(E)-1-(2-pyridyl)-2-styryl-1H-benzimidazoleHCID 12542153(E)-3-cyclohexylacryloyl chlorideHCID 227367644-methyl-2-amino-N-(2-pyridyl)aniline

생성물 1

HCID 9953200(E)-2-[2-(Cyclohexyl)ethenyl]-5-methyl-1-(2-pyridyl)-1H-benzimidazole oxalate

시약·촉매·용매 1

HCID 8857
Ethyl Acetate
용매

실험 절차

Free base of the titled compound was prepared from 4-methyl-2-amino-N-(2-pyridyl)aniline and (E)-3-cyclohexylacryloyl chloride according to the preparation of (E)-1-(2-pyridyl)-2-styryl-1H-benzimidazole (Example 1, method A). The free base and oxalic acid were dissolved into ethyl acetate. Concentration and recrystallization from ethyl acetate/n-hexane yielded the titled compound.

후처리

  1. concentrationConcentration and recrystallization from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-b74d7f3878744020a119c44a07c44119
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310079B1

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