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Diisopropylethylamine → 3,6-dichloro-N-(2,3-difluorobenzyl)-1,2,4-triazin-5-amine

HRID 577426
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HRID 577426 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[C:6](Cl)[N:7]=1.[F:10][C:11]1[C:18]([F:19])=[CH:17][CH:16]=[CH:15][C:12]=1[CH2:13][NH2:14].CCN(C(C)C)C(C)C>CN1C(=O)CCC1.CCOC(C)=O>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[C:6]([NH:14][CH2:13][C:12]2[CH:15]=[CH:16][CH:17]=[C:18]([F:19])[C:11]=2[F:10])[N:7]=1
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참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 27369412,3-DifluorobenzylamineHCID 122624033,5,6-Trichloro-1,2,4-triazine

생성물 1

HCID 867064193,6-dichloro-N-(2,3-difluorobenzyl)-1,2,4-triazin-5-amine

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

3,5,6-Trichloro-1,2,4-triazine (520 mg, 2.8 mmol) was dissolved in 5 mL NMP. To it was added 2,3-difluorobenzylamine (0.36 mL, 3.1 mmol) and DIEA (0.54 mL, 3.1 mmol). The mixture was stirred at RT for 20 m. It was diluted with EtOAc, washed with brine twice, dried over MgSO4, concentrated in vacuo, and subjected to flash column to afford 3,6-dichloro-N-(2,3-difluorobenzyl)-1,2,4-triazin-5-amine.

후처리

  1. washwashed with brine twice
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f8ebd8b6dd44423b9befa333174a86eb
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040530B2

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