1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 71247910, 화합물

HRID 530913

반응식

HRID 530913 반응식
[I:1][C:2]1[CH:3]=[C:4]([NH2:10])[C:5]([NH:8][CH3:9])=[CH:6][CH:7]=1.[Cl:11][C:12]1[C:13]([C:18](O)=O)=[N:14][CH:15]=[CH:16][CH:17]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>O.N1C=CC=CC=1>[Cl:11][C:12]1[C:13]([C:18]2[N:8]([CH3:9])[C:5]3[CH:6]=[CH:7][C:2]([I:1])=[CH:3][C:4]=3[N:10]=2)=[N:14][CH:15]=[CH:16][CH:17]=1

참가 물질

7

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 8246323-Chloropyridine-2-carboxylic acidHCID 660642804-Iodo-N1-methylbenzene-1,2-diamine

생성물 1

HCID 71247910HCID 71247910, 화합물수율 73.4%

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

반응 조건

온도
100 °C

실험 절차

A mixture of 4-iodo-N1-methyl-benzene-1,2-diamine (850 mg), 3-chloro-pyridin-2-carboxylic acid (590 mg), WSC (790 mg), HOBt (46 mg), and pyridine (10 ml) was stirred at 100° C. for 12 hours. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2-(3-chloro-pyridin-2-yl)-5-iodo-1-methyl-1H-benzimidazole (930 mg), which is hereinafter referred to as “intermediate compound (M6-21)”.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c8ba6e03cd7f44a28e1ac82f19806503
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353110B2

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