1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 3-Chloropyridin-2-carboxylic acid (2-mercapto-5-trifluoromethylpyridin-3-yl)-amide

HRID 530908

반응식

HRID 530908 반응식
[NH2:1][C:2]1[C:3]([SH:12])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[Cl:13][C:14]1[C:15]([C:20](O)=[O:21])=[N:16][CH:17]=[CH:18][CH:19]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>O.N1C=CC=CC=1>[SH:12][C:3]1[C:2]([NH:1][C:20]([C:15]2[C:14]([Cl:13])=[CH:19][CH:18]=[CH:17][N:16]=2)=[O:21])=[CH:7][C:6]([C:8]([F:9])([F:11])[F:10])=[CH:5][N:4]=1

참가 물질

7

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 8246323-Chloropyridine-2-carboxylic acidHCID 178507667HCID 178507667, 화합물

생성물 1

HCID 1785221603-Chloropyridin-2-carboxylic acid (2-mercapto-5-trifluoromethylpyridin-3-yl)-amide수율 58.2%

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

A mixture of 3-amino-5-trifluoromethylpyridin-2-thiol (0.45 g), 3-chloropyridin-2-carboxylic acid (0.39 g), WSC (0.67 g), HOBt (31 mg) and pyridine (4 ml) was stirred at room temperature for 12 hours. To the reaction mixture was added water, and the mixture was filtered to collect a solid. The resulting solid was washed with water, followed by n-hexane, and dried to give 3-chloropyridin-2-carboxylic acid (2-mercapto-5-trifluoromethylpyridin-3-yl)-amide (0.45 g), which is hereinafter referred to as “intermediate compound (M20-11)”.

후처리

  1. filtrationthe mixture was filtered
  2. customto collect a solid
  3. washThe resulting solid was washed with water
  4. customdried

출처 및 근거

ORD 기록
ord-5fa5fde9cc70490bbc94a6f6946b5b98
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353110B2

연결된 노트

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